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Pre-lab Lecture

Distillation (Group Exp#1)


BACKGROUND READING:
Techniques Weights and Measure, Distillation
Videos Basics of Using a Balance, Distillation Simple, Distillation - Fractional

Laura Pavelka
laura.pavelka@mcgill.ca
CHEM 212

PRE-LAB CYCLE 1 - Distillation

Purification Techniques
Purification technique used depends on the nature of the material:

SOLIDS

LIQUIDS

RECRYSTALLIZATION, CHROMATOGRAPHY

DISTILLATION, CHROMATOGRAPHY

Distillation purifies based on variable volatility


(boiling point) of compounds
also good for removing solvents from solutions
and separating liquid mixtures

CHEM 212

PRE-LAB CYCLE 1 - Distillation

Distillation
Boiling Point: temperature at which the vapour pressure equals atmospheric pressure
Pure X

Mixture of X + Y

Ptotal = Px

Daltons Law:
Ptotal = Px + Py
Raoults Law:
Px = PxNx
Py = PyNy

constant boiling temperature

CHEM 212

PRE-LAB CYCLE 1 - Distillation

Distillation
Boiling Point: temperature at which the vapour pressure equals atmospheric pressure
Pure X

Mixture of X + Y

Ptotal = Px

Daltons Law:
Ptotal = Px + Py
Raoults Law:
Px = PxNx
Py = PyNy

increasing boiling temperature

CHEM 212

PRE-LAB CYCLE 1 - Distillation

Overview Distillation Lab

PURPOSE: perform a simple distillation and a fractional distillation on an


unknown mixture of methanol and n-butanol and determine the
volume/molar composition of the mixture
CHEM 212

PRE-LAB CYCLE 1 - Distillation

1. Simple Distillation Set-up


grease glass joints

CHEM 212

PRE-LAB CYCLE 1 - Distillation

1. Simple Distillation Set-up


heating block
stir/hot plate

CHEM 212

PRE-LAB CYCLE 1 - Distillation

2. Performing Simple Distillation

CHEM 212

set hotplate to a medium heating (~60 C)


insulate flask with aluminum foil
modify heat setting as needed for steady boiling
wait until first drop of distillate to record
temperature

PRE-LAB CYCLE 1 - Distillation

2. Performing Simple Distillation


record temperature and distillate every
0.5 mL collected
increase heat as necessary to maintain
collection rate (1 drop/5 seconds)

Volume Distillate
(mL)
0

CHEM 212

PRE-LAB CYCLE 1 - Distillation

Temperature
(C)

3. Fractional Distillation Set-up


grease glass joints

CHEM 212

PRE-LAB CYCLE 1 - Distillation

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3. Fractional Distillation Set-up


heating block
stir/hot plate

CHEM 212

PRE-LAB CYCLE 1 - Distillation

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4. Performing Fractional Distillation

CHEM 212

set hotplate to a medium heating (~60 C)


insulate flask with aluminum foil
modify heat setting as needed for steady boiling
wait until first drop of distillate to record
temperature

PRE-LAB CYCLE 1 - Distillation

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4. Performing Fractional Distillation


record temperature and distillate every
0.5 mL collected
increase heat as necessary to maintain
collection rate (1 drop/5 seconds)

Volume Distillate
(mL)
0

CHEM 212

PRE-LAB CYCLE 1 - Distillation

Temperature
(C)

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5. Graphical Analysis (Report)


TOTALLY FICTICIOUS IDEAL DISTILLATION CURVES
Temperature as a Function of Distillate Volume
30
29.5

Temperature (C)

29
28.5
28
27.5

Simple Distillation

27

Fractional Distillation

26.5
26
25.5
25
0

0.5

1.5

2.5

Distillate Volume (mL)

CHEM 212

PRE-LAB CYCLE 1 - Distillation

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Safety & Waste Disposal


Special Safety Considerations:
Methanol Hazardous in case of skin/eye contact, inhalation/ingestion. Flammable.
n-Butanol Hazardous in case of skin/eye contact, inhalation/ingestion. Flammable.

Waste Disposal:
Methanol/n-Butanol Mixtures

CHEM 212

Non-halogenated organic waste

PRE-LAB CYCLE 1 - Distillation

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