Title: Experiment 4

INTRODUCTION TO A BATCH PROCESS: SIMPLE BATCH DISTILLATION

Objectives:
To separate an ordinary binary mixture consisting of acetic acid and water
using a sample batch distillation technique.

Apparatus:
Beaker, conical flask, measuring cylinder, Erlenmeyer flask, distillation kit,
hot plate, burette and volumetric flask.

Theory:
An ordinary binary mixture is a mixture which contains only two
components (A and B) that mixes at all proportion to form a homogeneous
solution. A denotes a much volatile component that has lower boiling
point or higher vapour pressure while component B is less volatile. By
utilizing their difference in volatility, we can separate these compartments
by heating the mixture. The vapour generated by the heating generally
has a higher content of component A while component B is normally
concentrated in the residual liquid. Hence, the separation has taken effect.
This separation is called distillation.
In this experiment, we will distil a mixture of acetic acid-water using a
simple batch technique whereby the generated vapour is condensed as
fast as it forms so that the vapour will not reach equilibrium with the
liquid. The mathematical treatment of this type of distillation is given in
the form of Raleigh equation.

Procedure:
A. Distillation
i. Prepare an acetic acid-water solution by adding 20ml acetic acid (sg
= 1.048) to 10 ml distilled water in Erlenmeyer flask (a conical flask
from the distillation kit).
ii.
Put the flask on a hot plate. Using apparatus supplied in the
distillation kit, set the solution up for distillation as demonstrated by

iii.

iv.
v.

vi.
vii.

instructor. Work gently since the glassware is quite fragile and

expensive.
Gently turn on the tap to let cooling water into the condenser. Make
sure that the hose for outlet water is inside the sink. Adjust the inlet
water rate so that the cooling water enters at a rate sufficiently
enough to cool and condense the vapour completely but not too
high as to render the equipment set up unstable.
Weigh a clean and dry 150ml beaker and position it beneath the
distillate outlet spout to collect the distillate.
Check and make sure all the connections fit snugly before the
distillation process begin. Start the distillation by turning on the hot
plate. The heating control switch should be positioned at 6 or 7.
When the solution inside the flask is approximately one-third
vaporized, turn off the hot plate.
Wait until the plate cools down and let all the vapours condense
before attempting to disassemble the distillation equipment. While
disassembling the glassware, be careful not to spill any distillate
that might be trapped in between the connections. You should
collect this trapped and add up to collecting beaker.

B. Titration of distillate
i. Reweigh the collecting beaker including its content.
ii.
Pour all distillate from the beaker into a 250ml volumetric flask.
Wash into the flask the remaining distillate left on the beaker wall
with distilled water.
iii.
Fill half of the flask with distilled water. Put its cap and shake the
flask gently a few times. Then fill up the flask up to the mark with
distilled water. Put the cap on again and turn the flask upside down
a few times so that the solution is well mixed.
iv.
Pour about 100ml of the diluted solution into a clean beaker. Using a
pipette, take 20ml or 25ml of the diluted solution each into 3
separate clean conical flasks. Then squeeze 2 drops of
phenolphtalein indicator into each flask.
v. Fill a burette with 1.0M of NaOH solution and titrate the content of
each flask with NaOH.

C. Titration of liquid residue

i. Repeat steps B1 to B5 for the liquid residue.

: Distillation with the standard macro scale lab kit.

Result:
Distillation
Volume

Mass (g)

Mole (g/mol)
10.6639
30

20ml of acid

Mole fraction
0.186065
0.47128

10.6639

39.4
= 0.1777
5.1440
18

10ml of water

= 0.3940
0.245200
0.47128

5.1440

52.02
= 0.2858

=0.5203

Balanced equation:
CH3COOH + NaOH

CH3COONa + H2O

MaVa a
=
MbVb b

Residue: Number of Mole of A

Measuring of NaOH distillate

Measuring of NaOH residue

Reading 1

13.0

Reading 1

22.8

Reading 2

10.4

Reading 2

23.0

Reading 3

10.0

Reading 3

22.6

Residue
Solution

Acid

Mass (g)

10.5739

Mol (g/mol)
10.5739
60
= 0.1762

Mole fraction

0.1762
0.5969
= 0.2952

29.55

NaOH

16.3424

16.3424
40
= 0.4086

0.4086
0.5969
= 0.6845

68.45

Solution

Acid

Mass (g)

5.46270

Mol (g/mol)
5.46270
60

0.0910
0.5117

= 0.0910

=0.1779

16.8424
60
NaOH

Calculation:
: Distillate
MaVa a
=
MbVb b
Ma(20)
1
=
( 1.0 ) (11.30) 1
Ma=

11.30
20

Ma=0.5565

: Residue
MaVa a
=
MbVb b
Ma (25)
1
=
( 1.0 ) (22.80) 1
Ma=

22.80
25

Ma=0.9120

16.8424

Mole fraction

= 0.42106

17.78

0.42106
0.5117
=0.8228

82.28

No of mole of A = [ ] = mole/volume
0.5565 = mole / (20/1000)
= 0.0113 mole of acid

No of mole of B = [ ] = mole / volume

0.9130 = mole / (25 / 1000)
= 0.0288 mole of base

Discussion:
Based on the experiment, the one that was distilled was water and acid
was the residue left in the distillating flask. But they might be traces of
acid in receiving flask and water in distillating flask. This experiment need
to be handle with care and careful due to the apparatus that quite
expensive and fragile.
Based on the result, there might be an error to the reading of acid and
water. After the distillation process, there is still water in the condenser
that was left. This may affect the reading of mass of water in the receiving
flask. Apart from that, some of evaporated water may be escaped from
the process due to the error in setting the apparatus. This can affect the
results.
In titration, thing that can affect the result is the way of handling the
burette during the experiment. There is a right technique to handle it. By
doing so, the result might be as accurate as possible.
In this experiment, we need to handle the apparatus and material
carefully as it quite fragile and rather expensive to replace. Apart from
that, we need to handle the experiment very carefully as if there any
small error, it may affect the whole results of the experiment.

Conclusion
The separation of ordinary binary mixture consisting of acetic acid and
water can be done by using a simple batch distillation technique.

References
Chemistry, 10th edition by Raymond Chang 2010
General Chemistry, 3rd edition by Daniel D. Ebbing