Distillation - Experimental Procedure

Aim
Set up a simple distillation column for an unknown mixture in order to separate into two purer
fractions. The boiling point of the purer fractions will then be measured and used to determine which
organic solvent they are.

Health & Safety
BASIC SAFETY RULES:

a) Do not eat, drink or chew whilst doing the experiment.
b) Keep your face at a safe distance from open flames and heated solutions. Never look into a
heated solution from above.
c) Avoid breathing in dust or vapor. When smelling solutions, gently wave the air above the
solution towards your nose with your hand.
d) Wash any spilled solutions from your skin with plenty of water, and notify the instructor.
e) Report any accident, no matter how minor, to the instructor/report the nearest health post.

The experiment involves heating liquids to their boiling point by use of a heating mantle. The heating
mantle may reach temperatures of 300
o
C and caution must be exercised in handling the heating mantel
and the equipment being heated. Low boiling point solvents may also be used and therefore must be
aware of the effects of rapidly heating such solvents or if solvents come into contact with a hot surface.

Procedure
1. Distillation
You will be given 30 ml of an unknown liquid mixture that is to be purified by simple distillation and
for which the boiling point range is to be determined.

1. Assemble the assigned distillation apparatus (consisting of the distillation flask, reflux
assembly, thermometer (up to 150
o
C), distillation arm, condenser attached to a water supply
and receiver) on a heating mantle using a heating block, ensuring that the reflux round bottom
flask (50 ml) contains 30 ml of the unknown liquid and a few boiling chips. Collection will be
made in a dry graduated cylinder at the receiver. The round bottom flask must be supported by a
clamp (do not over tighten). Clips must be used to support the remaining connections. The
thermometer must be placed where the bulb is positioned at the distillation arm. Do not seal the
system closed.
2. Check with the TA or Instructor that the assembly is ready.
3. The condenser is connected to a single water supply. Ensure only a gentle flow of water in the
system rapid flow of water may cause the leads to be ejected from the assembly and flooding.
4. Place the distillation flask in contact with the heating mantle ensure heating mantle is below
50
o
C cover the reflux assembly in aluminum foil just below the distillation arm.
5. Heat the unknown liquid gradually until the thermometer reaches a temperature around 50
o
C
then proceed at a slower rate till the vapor condenses and is collected at the receiver. As the
lower boiling point component is distilled, the boiling point of the mixture in the distillation
flask will increase.
6. Record the temperature at the first drop collected and for every 2 ml of liquid collected
thereafter.
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7. After 10 ml is collected, remove the cylinder and label Component A. Place another dry
cylinder underneath the receiver.
8. If the distillation flask is approaching dryness, remove the heat source immediately and contact
your TA or Instructor.
9. Collect the next 10 ml, recording the temperature after every 2 ml is collected. Towards the end
of the collection, the thermometer should reach a constant temperature.
10. Turn off the heating source. You must ensure the system is cool before touching it.
11. Once the system has cooled sufficiently, collect the residual liquid in the distillation flask and
label Component B.

2. Boiling point determination

1. Assemble the assigned boiling point apparatus (consisting of a heating flask with a side arm,
thermometer (up to 150
o
C), and a reflux condenser) on a heating mantle using a heating block,
ensuring that the heating flask contains at least 5 ml of Component A or B and a few boiling
chips. It is advised that you should test the boiling point of Component A first and then B. The
thermometer must be placed above the level of the liquid and not where the bulb contacts the
glassware. Do not seal the system closed.
2. Check with the TA or Instructor that the assembly is ready.
3. The condenser is connected to a single water supply. Ensure only a gentle flow of water in the
system rapid flow of water may cause the leads to be ejected from the assembly and flooding.
4. Place the heating flask in contact with the heating mantle ensure heating mantle is below 50
o
C.
5. Heat the Component liquid gradually until the system produces condensation on the
thermometer.
6. Record the temperature of the system.
7. Turn off the heating source. You must ensure the system is cool before touching it.
8. Repeat for the other Component liquid.

Result processing
Identify the unknowns by their boiling points using the possible boiling points of compounds.
Construct a table like that given below, to record the temperature at the distillation "head" as a function
of volume distilled. You will record your data in report form. Plot distillate temperature (
o
C) vs. volume
of distillate (ml) collected for the mixture and use the graph to determine the boiling points of the two
compounds in the mixture and identify the compound in the mixture.

Report Form

Volume distilled
(ml) 0 2 4 6 8 10 12 14
Temperature (oC)
Volume distilled
(ml) 16 18 20 22 24 26 28 30
Temperature (oC)



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Observed boiling point of the first compound (A): ____________oC
range
Literature boiling point of the first compound (A): ____________oC
range
Observed boiling point of the second compound (B): ____________oC
range
Literature boiling point of the second compound (B): ____________oC
range

Identity of Mixture
Compound A is _____________________
(name)
Compound B is _____________________
(name)

Identity of Mixture (Group 2)
BP for compound A _________oC; Compound A is _____________________
(name)
BP for compound B _________oC; Compound B is _____________________
(name)


Post-lab Questions

1. One mole of compound A, with vapor pressure 400 mmHg at 50 oC, mixed with 3 moles of
compound B, with vapor pressure 480 mmHg at 50 oC to form a homogeneous solution. What is
the vapor pressure of mixture at 50 oC?
(1 mark)

2. Why should a distilling flask be filled not less than 1/3 filled or more than 2/3 full?
(1 mark)

3. A 50% aqueous solution of ethanol (50 ml total) is distilled and collected in 10ml fractions.
Predict the boiling range of each fraction.
(2.5 marks)

fractions vol. collected(ml) temp. oC (predicted)
1 10
2 20
3 30
4 40
5 50

4. What is the mole fraction of each component if 3.9 g of benzene (C
6
H
6
) is dissolved in 4.6 g of
toluene (C
7
H
8
)?
(2 marks)

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5. Define the following terms.
(3 marks)
Reflux -
Daltons Law -
Raoults Law

6. Why should you never seal (close) a heated reaction without specialist glassware?
(1 mark)

7. What is the purpose of boiling chips in a simple distillation experiment? Why should you not use
them for larger reaction vessels or larger quantities of mixture?
(1.5 marks)

8. Briefly explain the chemistry involved in the fractional distillation of crude oil, using an atmospheric
distillation unit as an example.
(3 marks)

Submission
You will need to submit a lab report writing-up your experiment, data and results. This must include
the post-lab questions at the end of the report.

The lab report must be handed in 2 weeks from the date of your lab class, no later than 5pm.
Reports must be submitted electronically through Moodle. Reports must be typed on a computer and
not a scanned handwritten report. Late submission will be penalized.

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