NAME: Machell Lee

ID #: 05714408

LABORATORY EXERCISE: BD
LAB TITLE: Batch Distillation
GROUP: B2
DEPARTMENT: Chemical Engineering
DATE PERFORMED: February 7, 2006
DATE SUBMITTED: February 14, 2006

Abstract
The aim of this experiment was to (1) chart the operation of a simple distillation
operation and compare it with relevant theory and (2) compare a batch rectification
operation with a simple distillation.
A 1:1 ethanol-water mixture was distilled via simple and fractional distillation.
The time to collect successive 30cm3 portions of distillate was measured until 150 cm3
was collected. The temperature and density (using pycnometers) were measured on each
occasion and the mass fraction of the more volatile component (ethanol) in each was
determined. A graph of mass fraction against time was plot for both distillation processes
and their results compared.
Using the presented theory and the relevant experimental results the mole fraction
of ethanol in the distillate and in the waste were calculated for both processes. Fractional
distillation delivered a distillate of greater ethanol concentration. Fractional distillation
resulted in a fairly constant high mole fraction of ethanol in the distillate, which
emphasizes its efficacy as a separation process; while the less effective simple distillation
resulted in the smaller ethanol mole fraction decreasing with time.

Introduction
Distillation is a technique used to separate a mixture of two or more liquids. The
mixture is boiled and the vapour condensed and collected as distillate. Since the vapour is
richer than the liquid in the more volatile component the distillate will also richer in the
more volatile component since it has the same composition as the vapour being
condensed.
In batch distillation (differing from continuous distillation) the liquid is held
within the distilling flask while the distillate is continuously taken off. The original
distillate will have the highest concentration of the more volatile component (ethanol) but
this gradually decreases as its concentration in the liquid decreases. There are two types
of batch distillation: Simple and Fractional distillation.
In simple or differential distillation the vapour is directly condensed as it leaves
the flask and at any given time the vapour is in equilibrium with the liquid in the flask.
Since the concentration of both the liquid and vapour is changing, the process is a time
dependent one. However, if a rectifying column is installed (fractional distillation) a
continuous distillation of the liquid mixture occurs. As the vapour rises in the
fractionating column it is repeatedly condensed and vapourised. Since the vapour
becomes richer in the more volatile component at each instant, this results in a greater
concentration of product being formed. Also the distillate composition does not vary with
time. Thus, the latter is the more effective in separating mixtures.

Experimental
Apparatus and Chemicals

Electrical muffle heater

2 Round bottom flasks

Thermometer

Condenser

Measuring Cylinders

6 Pycnometers (density bottles)

Fractionating Column

Beaker

Ethanol

Distilled water

Procedure
1. The apparatus for simple distillation was set up.
2. The mass of the six pycnometer bottles, with their corresponding covers labelled
1-6 were measured.
3. A 1:1 mixture of water and ethanol was prepared in a round bottom flask using
125 ml of each solution.
4. The density of this mixture was determined by measuring the combined mass of
the mixture in the pycnometer, the vessel and the cover.
5. This known mass of feed was charged to the system.
6. The heater was put on maximum rate and cooling water put on the condenser.
7. The condensate was collected in a measuring cylinder and the timer started when
the first drop of condensate fell into the cylinder.
8. The time was noted at every 30 ml of condensate collected.
9. Each 30 ml sample was collected separately in a measuring cylinder and its
density measured using the pycnometer.

10. The temperature of each sample of condensate was also noted.

11. The experiment was stopped when 150 ml of distillate was collected.
12. The temperature and density of the bulk distillate was noted.
13. The residue was left to cool to a suitable temperature when its density was
determined.
14. A fractionating column was attached to the equipment and steps 3-13 repeated for
fractional distillation.

Analysis and Presentation of Results

m1 - mass of pycnometer and cover
m2 - mass of sample with pycnometer and cover
m3 - mass of sample only
Volume used = 25 ml

Sample Calculation
(Using initial reading from simple distillation)
m3 = m2 - m1
= 50.4 28.2 = 22.2 g
Density =

mass
22.2

volume
25

= 0.888 gcm-3
Mass of feed, F = density x volume
= 0.888 x 250 = 222 g
Mass fraction ethanol = 58.48% (using composition table)
Mass of ethanol = 222 x 0.5848 = 129.8256 g
Moles of ethanol =

129.8256
2.821069mol
46.02

Mass of water = 222 129.8256 = 92.1744 g

Moles of water =

92.1744
5.115117 mol
18.02

Total moles = 2.821069 + 5.115117 = 7.936186

Mole fraction ethanol, xf =

2.821069
= 0.355469
7.936186

Mass of distillate, D = 127.8 g

Mass fraction ethanol = 73.65% (using composition table)
Mass of ethanol = 127.8 x 0. 7365= 94.1247g
Moles of ethanol =

94.1247
2.0453mol
46.02

Mass of water = 127.8 94.1247 = 33.6753g

Moles of water =

33.6753
1.868774mol
18.02

Total moles = 2.0453 + 1.868774 = 3.914073

Mole fraction ethanol, yD,av =

2.0453
= 0.52255g
7.936183.9140736

W = F D = 222 - 127.8
= 94.2 g
Mass fraction ethanol = 39.48% (using composition table)
Mass of ethanol = 94.20 x 0.3948 = 37.19016 g
Moles of ethanol =

37.19016
0.80813mol
46.02

Mass of water = 94.2 37.1906 = 57.00984 g

Moles of water =

57.00984
3.163698mol
18.02

Total moles = 0.80813 + 3.163698 = 3.971828

Mole fraction ethanol, xw =

0.80813
= 0.203466
3.971828

Table of results for simple distillation

Time (s) m1 (g) m2 (g) m3 (g) density (gcm-3) Temperature (oC)

Feed

mass fraction

28.2

50.4

22.2

0.888

33

58.48

184.84

29.3

49

19.7

0.788

28

98.19

182.03

28

48.1

20.1

0.804

28

92.59

192.39

26.5

47.3

20.8

0.832

28

81.81

537.17

29

49.8

20.8

0.832

28

81.81

484.19

27.9

49.4

21.5

0.86

28

70.33

Distillate

28.2

49.5

21.3

0.852

28

73.65

Waste

29.3

52.5

23.2

0.928

31

39.48

mass feed (g)

mass ethanol (g)
moles ethanol
mass water (g)
moles water
total moles
mole fraction
ethanol

222
129.8256
2.821069
92.1744
5.115117
7.936186
0.355469

mass distillate (g)

127.8
mass ethanol (g)
94.1247
moles ethanol
2.0453
mass water (g)
33.6753
moles water
1.868774
total moles
3.914073
mole fraction ethanol 0.52255

mass waste (g)

mass ethanol (g)
moles ethanol
mass water (g)
moles water
total moles
mole fraction ethanol

94.2
37.19016
0.80813
57.00984
3.163698
3.971828
0.203466

Table of results for fractional distillation

Feed

Distillate
Waste

Time (s)
0
207.13
202.6
215.93
252.65
377.57

m1 (g)
29.3
28
26.5
29
27.9
28.2
28
26.5

m2 (g)
50.7
47.8
47
49.2
48.3
49.8
48.3
50.8

m3 (g)
21.4
19.8
20.5
20.2
20.4
21.6
20.3
24.3

density (gcm-3)
0.856
0.792
0.82
0.808
0.816
0.864
0.812
0.972

mass feed (g)

mass ethanol (g)
moles ethanol
mass water (g)
moles water
total moles
mole fraction ethanol

214
150.1852
3.263477
63.8148
3.541332
6.804809
0.479584

mass distillate (g)

mass ethanol (g)
moles ethanol
mass water (g)
moles water
total moles
mole fraction ethanol

121.8

mass waste (g)

109.352
2.376185
12.44796
0.690786
3.066971
0.774766

92.2
mass ethanol (g)
12.61296
moles ethanol
0.274076
mass water (g)
79.58704
moles water
4.416595
total moles
4.690671
mole fraction ethanol 0.05843

Temperature (oC)
33
28
28
28
28
28
27.5
33

mass fraction
70.18
96.84
86.55
91.12
88.1
69.02
89.78
13.68

Representation of results

Simple
Distillation
Fractional
Distillation

Mole Fraction
Ethanol In Feed
xf

Mole Fraction
Ethanol In
Distillate
yDtavg

Mole Fraction
Ethanol In Residue
xw

0.355469

0.52255

0.203466

0.479584

0.774766

0.05843

Comparison with Theoretical Data

Simple Distillation

dL x dx
x
W L
y * x
F

Upon integration this equation gives ln

F
which is equal to the area under the curve
W

x vs. 1/(y*-x) curve, between the limits xw and xf,

where F is the total number of moles in the feed, and
W is the total number of moles in the waste
7.936186 = ln 1.9981
F

3.971828
W

ln

= 0.6922
Comparing with:
Area of graph between xf and xw = 10.5 blocks x area of block
= 10.5 x 0.05
= 0.525 units2

Discussion
The first distillate from the simple distillation was found to be the highest in
concentration of ethanol (98.19 % by mass) and higher than that of the starting mixture
(58.48%) - as would be expected from the theory. As time increases however, there is a
gradual decrease in the concentration of ethanol in the distillate, that is, the composition
of the vapour was continuously changing with time. This proves that batch distillation is a
time dependant or unsteady process.
The graph for fractional distillation shows that the initial distillate was higher in
ethanol concentration than the original mixture (96.84%), as expected, but thereafter the
value remained fairly constant with some fluctuations. There was thus no obvious
relationship between the composition of the more volatile component (ethanol) in the
distillate and time; hence the composition did not vary with time.
The mole fraction of ethanol in the bulk distillate was higher for fractional
distillation (0.774766) than for simple distillation (0.552255) (similarly, the mass %)
therefore proving that fractional distillation provides a more effective separation of the
components in the mixture.
Since the aim of the experiment was simply to compare the two distillation
techniques, it was not necessary to completely separate the two liquids. Nevertheless,
neither of these two distillation methods would be able to fully carry out such a
separation because the ethanol-water mixture is a homogeneous azeotropic one, which
can only be separated by azeotropic distillation.
The change in the number of moles calculated from the experiment is similar to
that from the relevant theory with only a difference of (0.1672). Precautions were taken
throughout the experiment to ensure accuracy of results. These include ensuring that each
pycnometer was covered with the same cover each time to prevent any variations in mass
and hence the values calculated. Another precaution taken was to ensure that there was a
continuous flow of water in the condenser so that there were no bubble spaces to hamper
the condensation process.
However, this difference may have resulted from errors in the readings, and/or
experiment from assumptions or approximations. Possible sources of errors are:

1) The assumption that there was no loss in volume of the distillate when losses
occurred when switching measuring cylinders and measuring the densities
using the pycnometer.
2) Reaction time in starting and stopping the stopwatch.
3) The approximation involved in the counting squares method of determining
the area underneath the curve.
4) Improper securing of the connections in the apparatus which could have
caused vapour to escape into the surroundings.
5) Incomplete stirring or mixing of the original mixture which may have resulted
in a greater concentration of ethanol being on the surface or bottom of the
flask.
The experiment could have been improved by insulating the columns so
preventing heat loss and by placing petroleum jelly over the joints to ensure that
no vapour escapes the apparatus.

Conclusion

The mole fraction and (mass fraction) of ethanol in the distillate was higher
for fractional distillation than simple distillation.

The distillate produced from simple distillation was highest in concentration

of the more volatile component initially, and then decreased with time. Thus
simple distillation is a time dependent process.

Ethanol composition in the distillate produced from fractional distillation is

constant with time (independent of time).

Fractional distillation is a better separator of an ethanol-water mixture as it

results in a purer distillate being formed.

For simple distillation the change in the number of moles in the experiment
was approximately the same as that from the theory.

Refrerences

THE UNIVERSITY OF THE WEST INDIES Laboraory Manual CH11A

Applied Chemistry I and CH17B Chemical Engineering Laboratory I (20052006)

McGAW, D.R.; MELLOWES, W.A.; YOUNG HOON, A. and FARABI, H.

Introduction to Chemical and Process Engineering

CHOPEY, M.P. Handbook of Chemical Engineering Calculations. Td Edition

1994, Mcgraw Hill