Simple (Expt. 5) & Fractional Distillation (Expt. 6)
SAFETY
See page 53-55 in textbook. Figure 2.37(a) is the setup for simple distillation. Substitute a graduated cylinder as
the receiving flask rather than the round bottom flask.
Never heat a system that is totally closed from the outside atmosphere, as an explosion is likely to occur.
Never heat a system to dryness because of possible explosion!!!
Procedure
**Get your apparatus set up as quickly as possible and begin distillation!!
Simple Distillation
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Heating mantle with variac
Lab jack (or a ring clamp)
25-mL round bottom flask
Boiling chips
Condenser
Thermometer – make sure it’s a CELSIUS thermometer!! (not Fahrenheit)
Distillation Head
(vacuum) adapter – we are not using a vacuum, but need this connection for our setup
3 labeled vials and caps
2 graduated cylinders for collection of distillate
Sand
Keck clips, clamps, ring stand
For Fractional Distillation, add a Vigreux column between stillpot and stillhead. Wrap it with Al foil.
Follow directions carefully.
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Set up the apparatus. Be sure to position the thermometer in the stillhead so that the top of the mercury
thermometer bulb is level with the bottom of the sidearm of the stillhead! Make sure that you clamp the
neck of the round bottom flask (the stillpot) to the ring stand--do NOT use a Keck clip!!
Be sure you put 1-2 boiling stones into the stillpot.
Add 10 mL of a mixture of ethyl acetate and butyl acetate to the stillpot. (Note the ratio of the ethyl
acetate to butyl acetate mixture in your data & observations section.)
Make sure all joints are lightly greased and properly seated so that there are no vapor leaks. (Don’t go
crazy with the grease, b/c most glass joints will have residual grease on them from the class before. If
you use too much grease, it will get into your acetate mixture and contaminate it.)
Make sure the water is running through the condenser with no water leaks BEFORE YOU START
HEATING!!!
Have the instructor check your setup before you start heating!!
Have 2 small graduated cylinders in which to collect the distillate and three properly labeled bottles to
hold the fractions you collect.
Heat the mixture to a boil. When the distillate begins to drip off the thermometer, check the drip rate. If
you heat the solution too fast, you will not achieve separation. The drip rate should not be faster than
one drop every 3-5 seconds.
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Watch for the first drop of distillate to come out of the condenser and then begin to monitor temperature
and volume of distillate.
When you have 1 mL of distillate in the graduated cylinder, record the temperature on the thermometer.
Continue to record the temperature as each additional milliliter is collected.
When you have collected the first 3 mL of distillate, switch to the second graduated cylinder and
continue to collect distillate and record temperature. Place the collected distillate in a vial labeled
sample #1. Clean the 1st graduated cylinder for use again.
When you have collected the next 3 mL, switch to the clean graduated cylinder and continue to collect
distillate and record temperature every 1 mL. Place the 2nd volume of collected distillate into a vial
labeled sample #2.
When you have collected the last 3 mL (DO NOT LET THE ROUND BOTTOM FLASK GO DRY) in
the graduated cylinder, turn the heating mantle off. Place the collected 3 mL in vial labeled sample #3.
DO NOT disconnect the apparatus until it has cooled.
When the “pot” is cooled, collect the residue in the “pot” and add it to the third vial labeled sample #3.
Store your samples as instructed.
Clean your lab space and properly dispose of any chemical waste.