Simple and Fractional Distillation
Expt. #4 & #5 will be done on the same day -- HALF OF THE STUDENTS WILL DO
SIMPLE AND HALF WILL DO FRACTIONAL. (You will do either simple or fractional,
and your hoodmate will do the other one!!) Everyone needs to have their own notebook
prepared for lab. You will share your data with your hoodmate at the end of lab, so that you
both have the data for simple and fractional distillation.
SAFETY
 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 – Hand write the procedure into your notebook!!!
Get your apparatus set up as quickly as possible and begin distillation!!
Materials:
Heating mantle & variac
Lab jack
Vigreux column -- (for fractional distillation set up ONLY)
25-mL round bottom flask
Boiling chips
Condenser
Thermometer
Distillation Head
Graduated cylinder for collection of distillate
3 vials and caps
2 graduated cylinders
Keck clips (yellow)
Labels
Follow directions carefully.
1.
2.
3.
4.
5.
6.
Set up the apparatus.
Be sure you put 1-2 boiling stones into the “stillpot”.
A 10 mL of a mixture of ethyl acetate and butyl acetate will be used. Add the mixture to the “pot”.
NOTE THE RATIO OF ETHYL ACETATE TO BUTYL ACETATE.
Make sure all joints are greased and properly seated so that there are no vapor leaks.
Make sure the water is running through the condenser with no water leaks.
Have 2 small graduated cylinders in which to collect the distillate and four properly labeled bottles to
hold the fractions you collect.
7.
8.
9.
10.
11.
12.
13.
14.
15.
17.
18.
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 off of the thermometer
should not be faster than one drop every 3-5 seconds.
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 mL 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 next 3 mL (DO NOT LET THE ROUND BOTTOM FLASK GO DRY) in
the graduated cylinder, turn the heating mantle off. Place collected 3 mL in vial labeled Sample #3.
(When there is not enough liquid in the “pot” to be distilled, the temperature will drop.)
DO NOT disconnect the apparatus until it has cooled.
When the “pot” is cooled, collect the residue in the stillpot 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.