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SAFETY: Phosphoric acid is corrosive. Causes severe skin burns and eye damage - handle with care.
Step 2. Add phosphoric acid (conc.)
Step 2. Add phosphoric acid (conc.)
Good call! Add the phosphoric acid (conc.) and one boiling chip before assembling the apparatus.
1.2.mp4Discuss: Why is it sensible to use acid-catalysis for dehydration reactions?
Step 3. Start warming up the sand bath! ~medium
Step 3. Start warming up the sand bath! ~medium
SAFETY: HOT! Do not leave thermometer in sand bath. Surroundings should be free from clutter.
Step 4. ASSEMBLE!
Step 4. ASSEMBLE!
Use small amount of grease for glass connections.
<---- condenser
<--- Hickman Still
<--- Keck clip (yellow)
<--- 5 mL RBF
(with starting reagents + boiling chip)set-up.mp4Step 5. Start distilling!
Step 5. Start distilling!
Check the temperature of the sand bath, target temp. = 150 – 170°C
Secure apparatus using a clamp and ring stand
Hook up water lines for condenser: blue (cold, in) = bottom
Add hose clamps to secure lines to condenser!
Turn on water flow by loosening the clamp blocking the lines
distillation.mp4*disclaimer: hard to see the product collecting in the Hickman still in this video*
As the reaction occurs, the alkene products that form will distill and collect into the Hickman still, driving the equilibrium to the right to make even more products...keep a careful eye on the amount of liquid remaining in the flask!
After ~10 minutes, the ring of the Hickman still looks like this...
What should you do?
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