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Lab#5 - Separation and Purification of Organic Liquids by

Distillation
March 4, 2015
Submitted to: Kevin
Submitted by: Taylor Sanderson
Lab Partner: Chloe Van Der Cruysen

Lab#5 -

Separation and Purification of Organic Liquids by Distillation

Purpose
The main objective in this lab is to first distill a pure liquid and observe its constant
boiling point. Then you will distill a two component mixture twice once using a
simple distillation apparatus and then using a fractioning column. This will make it
able to compare the efficiency of these two types of apparatus by evaluating the
separation of the mixtures.
Procedure
For full procedure refer to Organic Chemistry 1 manual, experiment 5, Separation
and Purification of Organic Liquids by Distillation , Page 29-34.
Reagents
Hexane (C6H14)
Molecular weight:86.13 amu
Colour: colourless
Physical appearance: liquid
Melting point:-95C
Boiling point:69C
Toluene (C7H8)
Molecular weight:92.14 amu
Colour: colourless
Physical appearance: liquid
Melting point: -95C
Boiling point:111C
*Reference MSDS*
Equipment
Simple distillation apparatus
Distilling flask
Thermometer
Condenser
Adaptor
Graduated receiver
Boiling stone
250ml flask
Fractioning column
500ml round bottomed flask

Observations

Exercise A: Simple Distillation


Temperature
58C
59C
61C
61C
61C
61C

Number of Drops
1 drop/ml
3 drop/ml
5 drop/ml
7 drop/ml
9 drop/ml
11 drop/ml

Exercise B: Separation of a Binary Mixture by Simple Distillation


Volume (ml)
Temperature
Volume (ml)
Temperature
2ml
45C
28ml
70C
4ml
50C
30ml
68C
6ml
60C
32ml
71C
8ml
70C
34ml
74C
10ml
71C
36ml
76C
12ml
71C
38m
78C
14ml
73C
40ml
81C
16ml
76C
42ml
85C
18ml
74C
44ml
88C
20ml
73C
46ml
90C
22ml
75C
48ml
91C
24ml
73C
50ml
91C
26ml
71C
Exercise C: Separation of
Amount
Temperatur
(ml)
e
5ml
65C
10ml
68C
15ml
69C
20ml
71C
25ml
72C
30ml
73C
35ml
73C
40ml
74C
45ml
75C

a Binary mixture using Fractional Distillation


Amount
Temperatur
Amount
Temperatur
e
e
50ml
75C
95ml
82C
55ml
76C
100ml
84C
60ml
77C
105ml
85C
65ml
77C
110ml
85C
70ml
78C
115ml
85C
75ml
79C
120ml
86C
80ml
79C
125ml
86C
85ml
80C
130ml
88C
90ml
81C
135ml
92C

Discussion
The simple distillation is used to separate and purify liquids, if the temperature of
the liquid is raised, more molecules escape to the vapour until the equilibrium is
established. The vapour pressure of a liquid therefore increases with temperature.
Therefore this distillation has a constant boiling point. As shown in the graph on the
last page it shows the boiling point eventually being constant. It may have taken a
while to be constant due to some experimental errors during the lab. The constant
temperature for Hexane turned out to be around 61C. During the separation of
binary mixtures using simple distillation it seemed that the temperature was to high
on the apparatus to make the trend on the graph incorrect with the temperatures. It
seemed to be in the middle of the distillation that the temperature had dropped and

was suppose to be slowly increasing at all times. The average boiling point for
hexane and toluene using simple distillation turned out to be around 90C during
the distillation. During the separation of an binary mixture using fractional
distillation the separation did not seem to occur during the distillation and the
temperature was raising too quickly. The proper separation did not occur due to the
heat being too high at the beginning and it was causing the temperature to be off
by the binary mixture distillation happening to quickly resulting in inaccurate
results. According to the graph on the last page the temperature was raising too
quickly. The average boiling point for toluene and hexane during the fractional
distillation seemed to be around 86C. Referring to the results in the lab the simple
distillation seemed to be more efficient at separating the hexane and toluene
mixture.

Hexane Structure

Toluene Structure

Post Lab Questions


1. A pure liquid in a distilling flask does not vaporize all at once when the boiling
temperature is reached because the boiling point and vapor pressure hit equilibrium
and more heat will need to be applied(rise in temperature) to raise vapor pressure.
2. It is dangerous to heat a liquid in a distilling apparatus that is sealed tightly and
has no ventilation to the atmosphere because pressure in the apparatus will
increase to a high value and probably explode the distillation equipment.
3. A distilling flask should not filled to be more than two thirds of its capacity at the
beginning of a distillation procedure because in order to have room for the heat
expansion of the liquid and the forming vapours.
4. Some tests you could perform to make sure the separation happened between
toluene and hexane is TLC paper chromatography to see if you can see the
difference between the compounds separately and mixed together to see if they
separated after the distillation.
Conclusion
The Simple distillation worked more accurate during the separation of the binary
mixture and had a more accurate boiling point, 90C.

Simple Distillation (Exercise A)


62
61
60
Temperature (C) 59
58
57
56
0

10

12

# of Drops

Separation of a Binary Mixture Using Simple Distillation ( Exercise B)


100
80
60
Temperature(C)

40
20
0
0

10

20

30

Volume (ml)

40

50

60

Separation of a Binary Mixture Using Fractional Distillation (Exercise C)


100
90
80
70
60
Temperature (C) 50
40
30
20
10
0
0

20

40

60

80 100 120 140 160

Amount (ml)

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