I.

Separation of an ordinary binary mixture consisting of acetic acid and water by using
simple batch distillation technique.

II. Sample Experiment:

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a steam-jacketed-kettle and the vapor generated is withdrawn and condensed as fast as it forms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
to collect the distillate.
v 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
phenolphthalein was added into each flask.
v 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 Rough I I III

I

Final reading of the 20.80 20.60 20.30 20.00

burette (ml)

Initial reading of the 0.00 0.00 0.00 0.00

burette (ml)

Volume of NaOH (ml) 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 Rough I I III

I

Final reading of the 13.10 12.80 12.50 12.90

burette (ml)

Initial reading of the 0.00 0.00 0.00 0.00

burette (ml)
 Volume of NaOH (ml) 13.10 12.70 12.50 12.90

Average volume of NaOH: 12.70ml

V = 0.5943
Questions/Discussion ml

L1 =
0.9052 ml

XA =

L2 =
0.2199 ml

1. Calculate the molar composition of feed solution.

Species Volume(ml Mass(g) Mole(gmol Mole fraction Mole %

) )
20.98 0.3497
20 ×1.049 =0.3497 =0.38
HC2H3 20.0000 60 0.9052 38.63%
O2
10.00 0.5555
10 ×1.000 =0.5555 =0.61
H2O 10.0000 18 0.9052 61.37%

Total 30.0000 20.98 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 = ? Va = ?
Mb = 1.0 M 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 %

0.203
0.203 ×60=12. =0.342 0.342× 100=34.20
Acetic Acid 0.203 0.594

0.391
0.391× 18=7.0 =0.658 0.658 ×100=65.80
Water 0.391 0.594

Total 0.594 19.218 1.000 100.00

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

MaVa a
=
MbVb b

Ma = ? Va = ?
Mb = 1.0 M 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) Mole Fraction Mole %

0.1270
0.1270 ×60=7. =0.5775 0. 5775× 100=57.7
Acetic Acid 0.1270 0.2199
 0.0929
0.0929 ×18=1. =0. 4225 0. 4225 ×100=42.2
Water 0.0929 0.2199

Total 0.2199 9.2922 1.000 100.00

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

residual liquid. Compare the theoretical values with the experimental values.
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

III. Comparative Description

A. Procedure
Based on their experiment, an acetic acid-water solution was prepared in an
Erlenmeyer flask. The flask was put on heating mantle. The distillation apparatus was set up
as demonstrated. 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. A dry clean beaker was weighed and positioned
beneath the distillate outlet spout 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. The heating mantle was turned off after the solution inside the flask was approximately
one-third vaporized. 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. While based on our experiment, first we prepare a simple
distillation set-up and then we mixed 50-ml of glacial acetic acid and 1-ml of distilled water
in a 100-ml beaker. We pipet 1 ml of the mixture into each of two 125-ml Erlenmeyer flask
and label both flasks L-1 to make two trials then transferred the rest of the solution in step 2
to the distilling flask in the set-up and add the boiling chips. Slowly, we distilled the mixture
collecting the distillate in a clean, dry 10-ml graduated cylinder. Lastly, we read and recorded
the temperature when 3-ml of the distillate had been collected.

B. Materials
Their experiment was composed of Round bottom flask, Distilling head, Heating
mantle, Thermometer with adapter, Retort stamp with clamp, Condenser, Beaker,
Volumetric flask, Burette, Conical flask, Dropper, Pipette, Acetic acid, 1.0 M NaOH
solution, and Phenolphthalein. While our experiment was composed of distilling flask,
Erlenmeyer flasks, NaOH, Acetic acid and Phenolphthalein indicator.