| Steps
1-4 |
Photo |
Instructions |
| 1. Alcohol + H3PO4 |
(click here to learn
how to set up Hickman) |
Distill in
Hickman (microscale) apparatus |
| 2. Alkenes + H20 |
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Pipet
distillate from Hickman still head into the second
conical reaction vial using clean Pasteur pipet. •If you are not fully confident of your
pipetting technique, practice with a solvent such as
ethyl ether beforehand, but use a different pipet so as
not to contaminate the product.
•Note that it is the distillate
which is collected. The residue still in the vial is
properly disposed of.
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Note separate
layers of water and alkenes in vial. The bottom layer is
water, the top layer alkenes - you can see the curved
interface between them. If water adheres to sides, tap
the vial gently on bench. |
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Remove the
water layer with pipet and dispose of it; photo shows
this process at point where almost all of the water has
been removed. |
| 3. Alkenes + trace H2O |
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Dry over CaCl2 in 2-dram
vial with cap. Must stand for 24 hours or more to be adequately dried.
•Wrap
with plastic film (as shown below) to store the vial
until next lab period. The alkenes should be stored in
the refrigerator to reduce evaporation.
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| 4. Dry and store alkene
mixture |
©2001,2002 Daniel A. Straus
|
When dry,
pipet the solution into a second, clean tared 2-dram
vial. Wrap for storage as shown
and submit with your lab report.
Remember to do IR and GC analysis.
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