Steam Distillation
The purpose of this experiment is to demonstrate the ability to distill an organic liquid at a
temperature considerably below that of the boiling point of the pure liquid.
Procedure
Construct a steam distillation apparatus as set up in the lab.
Add your pulp and water to the distillation pot UNTIL HALF FULL.
Heat the mixture to a boil.
Note: Attempt to control the rate of heating so that excessive foaming does not occur.
At the first drop of distillate, record temperature and volume of distillate collected. Repeat this
every four mL, until 50 mL of distillate has been collected.
Stop the distillation. The distillate should have two layers. The top layer should be oil and
the bottom one should be aqueous. Transfer the distillate to a separatory funnel and allow the
mixture to stand for 5 - 10 minutes to allow complete separation. (See Figure above).
Drain off the aqueous layer.
Put the organic liquid (probably about 2 mL) in a clean, dry test tube and add a few granules
of anhydrous calcium chloride.
Measure the volume of the organic liquid (now dry).
Draw a Temperature vs Volume graph of your lab data in your lab report.
Test for unsaturation (multiple bonds between two carbon atoms):
a) Place one drop of cyclohexane in a depression of a white spot plate and add KMnO4
dropwise until a red-brown color persists for 30 seconds.
b) Place one drop of your distilled oil in another depression of a white spot plate, and add
KMnO4 dropwise until a purple color persists, or until you have added ten (10) more
drops to it than you added to the cyclohexane.
c) Record:
. the number of drops used for cyclohexane
. the number of drops for your oil, and whether or not a purple
color was reached
Turn in your product in an appropriately labeled narrow mouth bottle.
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Disposal of Spent Orange Peel
Construct a filtration apparatus as set up in the lab.
Place the piece of cheese cloth provided into your Buchner funnel.
Draw a vacuum on the funnel.
Pour the contents of your 500 mL round-bottom flask into the cheese cloth, and allow the
liquid to drain into the filter flask.
Once the liquid has been suctioned from the orange peel, discontinue vacuum and throw the
cheese cloth into the trash.
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Che 301
Su’2003
Lab Data Sheet
Title: Steam Distillation
Name:
Date:
Lab Data
Appearance of the liquid
( circle the appropriate description(s) )
Colorless color
cloudy clear
other comments
Volume of Liquid Used:
mL.
Temp. at which first drops enter the receiving vessel:
o
C
Volume/Temp Data
4 8
Vol
(mL)
12
16
20
24
28
32
36
40
44
48
52
56
Temp
(oC)
Volume of total distillate Recovered:
mL.
Volume of organic compound recovered:
mL.
. the number of drops of KMnO4 used for cyclohexane
. the number of drops for your oil, and whether or not a purple color was reached
(Y/N)
Che 301
Su’2003
Lab Report
Title: Steam Distillation
Name:
Date:
Results:(Draw Temp. vs Volume Graph)
Deg C
130
120
110
100
90
80
70
60
50
40
30
Volume (mL)
Convert the volumes of water and compound to moles utilizing
the information provided
Constituent
Molecular Weight (gm)
Density (g/mL)
Water
18
1.00
Citral
152.24
0.888
moles organic component =
In addition to the information asked for in the procedure, calculate the percent recovery in mL/l00gm
of starting material. Assume that the rind of six oranges weighs 80.0 gm.
Conclusion