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Abstract

In this experiment, the aim of this experiment is to separate an ordinary binary mixture
consisting of acetic acid and water using a simple batch distillation technique. Simple batch
distillation is also known as differential distillation refers to a batch distillation in which only
one vaporization stage is involved. This type of distillation is done boiling a liquid mixture in a
steam-jacketed-kettle and the vapor generated is withdrawn and condensed as fast as it
forms so that the vapor and the liquid do not have sufficient time to reach its equilibrium.
A mixture of acetic acid and water was used in this experiment. After the distillate was
collected about two third from the flask, it is then titrated with sodium hydroxide solution. It is
shown that the result of the titration has a slight different from each trial. From the results, we
can calculate the molar composition, composition of distillate and residual liquid, and the
theoretical composition of distillate as well as residual liquid.

Introduction/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 vapor pressure while component B is less
volatile. By utilizing their difference in volatility, we can separate these components by
heating the mixture. The vapor generated by the heating generally has a higher content of
component A while component B is normally concentrated in the residual liquid. Hence
separation is called distillation.
In this particular experiment, we will distill a mixture of acetic acid-water using a simple batch
technique whereby the generated vapor is condensed as fast as it forms so that the vapor
will not reach equilibrium with the liquid. The mathematical treatment of this type of distillation
is given in the form of Raleigh equation.

Objective
The aim of this experiment is to separate an ordinary binary mixture consisting of acetic acid
and water by using simple batch distillation technique.

Apparatus

Round bottom flask


Distilling head
Heating mantle
Thermometer with adapter
Retort stamp with clamp
Condenser
Beaker
Volumetric flask
Burette
Conical flask
Dropper
Pipette

Chemicals

Acetic acid
1.0 M NaOH solution
Phenolphthalein

Diagrams

Figure 3 (a) Distillation of acetic acid-water solution

Figure 3(b) Titration of distillate and liquid residue with NaOH solution

Procedure

A Distillation
i An acetic acid-water solution was prepared in an Erlenmeyer flask.
ii The flask was put on heating mantle. The distillation apparatus was set up as
demonstrated.
iii The tap was gently turned on to let the cooling water into the condenser. The inlet
water was adjusted so that the cooling water enters at a rate sufficiently high
enough to cool and condense the vapor completely.
iv A dry clean beaker was weighed and positioned beneath the distillate outlet spout
v

to collect the distillate.


The distillation was started by turning on the heating mantle. The heating mantle

control switch should be positioned at 6 or 7.


vi The heating mantle was turned off after the solution inside the flask was
approximately one-third vaporized.
vii The mantle was cools down and all the vapors were condensed. The distillation
equipment was disassembled. The trapped distillate was collected and added up
into the collecting beaker.
B Titration of distillate
i The collecting beaker including its content was reweighed.
ii All the distillate was poured into a 250ml volumetric flask. The remaining distillate
left on the beaker wall was washed with distilled water.
iii Half of the flask was filled with distilled water and was shaken gently a few times.
It then was filled up to the mark. The flask was turned upside down so that the
solution is well-mixed.
iv 100ml of the diluted solution was poured into a clean beaker. 25ml of the diluted
solution each then was pipette into 3 separate conical flasks. 2 drops of
v

phenolphthalein was added into each flask.


A burette was filled with 1.0M NaOH solution and the content of each flask was

titrated with NaOH.


C Titration of liquid residue
i The step B(i) to B(v) were repeated for the liquid residue.

Data/Result
Mass of beaker: 62.5558g
Mass of distillate: 81.7911g 62.5558g = 19.2353g
Mass of liquid residue: 71.8483g 62.5558g = 9.2925g
Table 3(a): Result of titration of the distillate

Trial

Final reading of the


burette (ml)
Initial reading of the
burette (ml)

Volume of NaOH (ml)

Rough

II

III

20.80

20.60

20.30

20.00

0.00

0.00

0.00

0.00

20.80

20.60

20.30

20.00

Average volume of NaOH: 20.30ml

Table 3(b): Result of titration of the liquid residue

Trial

Final reading of the


burette (ml)
Initial reading of the
burette (ml)

Volume of NaOH (ml)

Rough

II

III

13.10

12.80

12.50

12.90

0.00

0.00

0.00

0.00

13.10

12.70

12.50

12.90

Average volume of NaOH: 12.70ml

Questions/Discussion

L1 =
0.9052 ml
XA =
0.3863
XB

V = 0.5943
ml

L2 =
0.2199 ml

1. Calculate the molar composition of feed solution.

Species

Volume(ml)

Mass(g)

Mole(gmol)

HC2H3O2

20.0000

20.98
20 1.049=20.98 =0.3497
60

H2O

10.0000

10.00
10 1.000=10.00 =0.5555
18

Total

30.0000

20.98

0.9052

Mole fraction

Mole %

0.3497
=0.3863 38.63%
0.9052
0.5555
=0.6137 61.37%
0.9052
1.000

100.00%

Molar composition of the feed;


HC2H3O2
= 38.63%
= 0.3863
H2O
= 61.37%
= 0.6137
2. From the titration data, determine the composition of the distillate.
HC2H3O2 + NaOH
NaC2H3O3 + H2O

MaVa a
=
MbVb b

Ma = ?
Mb = 1.0 M

Va = ?
Vb = 20.30ml = 0.0203 L

MaVa
1
=
(1.0)(0.0203) 1
MaVa=( 1.0 ) (0.0203)
MaVa=0.0203 M 10=0.203 M
Composition of distillate:

Species

Mole

Mass(g)

Mole Fraction

Mole %

Acetic Acid

0.203

0.203 60=12.180

Water

0.391

0.391 18=7.038

Total

0.594

19.218

0.203
=0.342
0.594

0.342 100=34.20

0.391
=0.658
0.594

0.658 100=65.80

1.000

100.00

3. From the titration data, determine the composition of the liquid residue.

MaVa a
=
MbVb b
Ma = ?
Mb = 1.0 M

Va = ?
Vb = 12.70 ml = 0.0127 L

MaVa
1
=
(1.0)(0.0127) 1
MaVa=( 1.0 )( 0.0127 )
MaVa=0.0127 M 10=0.127 M

Composition of liquid residue:

Species

Mole

Mass(g)

Acetic Acid

0.1270

0.1270
=0.5775
0.1270 60=7.6200
0.2199

0. 5775 100=57.75

Water

0.0929

0.0929
=0. 4225
0.0929 18=1.6722
0.2199

0. 4225 100=42.25

Total

0.2199

9.2922

Mole Fraction

1.000

Mole %

100.00

4. Using Raleigh equation, calculate the theoretical composition of distillate and


residual liquid. Compare the theoretical values with the experimental values.
Solution:
By using Raleigh equation,

ln

L1
L2

0.3497

X2

where , ln

1
( y x
)dx

L1
=1.4
L2

To determine the value of x2, we can calculate the value between 0.35 and x2 must be
equal to 1.4.
After trial and error, at x=0.17 the area under the curve is close to 1.4
Thus, x2 = 0.17
From the result, the experimental value obtained are less than theoretical value, it is
caused by error while doing the experiment.

Conclusion
Separating acetic acid and water are possible by using simple batch distillation technique,
therefore, the purpose of this experiment achieved.

References
1. Pearson Longman,(2008),3th edition Chemistry of Basic Units,(p/g:178-185).
2. www.unit-operation-experiment-of-distillation.com// by Potter .L.(2005)/CHEMISTRY.
3. Experiment of simple batch distillation by John Burn(2001) 2nd edition.
4. Unit Operation 2, CMT203 by Azmi Mahmood and Mohamad Nizar Hassan, Module 3