UNIVERSITI TEKNOLOGI MARA, CAWANGAN PERLIS

KAMPUS ARAU

LABORATORY REPORT
CHM 450

EXPERIMENT 2 : SIMPLE BATCH DISTILLATION

DATE : 21 JUNE 2020
GROUP MEMBERS : ELMIRA ANNESSA BINTI ZAINUDDIN
(2020974807)
ISMAHANI BINTI ZAHUDDIN (2020974133)
LIYANA SYAKIRAH BINTI HASHIM
(2020993211)
NUR ALIYYA SYAKIRIN BINTI
SHAHARUDDIN (2020963781)
GROUP : AS245_2B
LECTURER :
OBJECTIVE :
The purpose of this experiment is to separate an ordinary binary mixture consisting of acetic
acid and water using a simple batch distillation technique.

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 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 has taken effect. This 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 an equilibrium with the liquid. The mathematical treatment of this
type of distillation is given in the form of Raleigh equation.

PROCEDURE :
A. Distillation
1. An acetic acid-water solution was prepared by adding 40 ml acetic acid (sg =
1.048) to 20 ml distilled water in an Erlenmeyer flask (a conical flask from your
distillation kit).
2. The flask was put on a heating mantel. Set the solution up for distillation by using
apparatus supplied in the distillation kit. Work gently since the glassware is quite
fragile and rather expensive to replace.
3. The tap was turned on gently to let cooling water into the condenser. Make sure
that the hose for outlet water is inside the sink. The inlet water was adjusted so
that the cooling water enters at a rate sufficiently high enough to cool and
condense the vapor completely but not too high as to render the equipment set-up
unstable.
4. A clean and dry 150 mL beaker was weighed and position in beneath the distillate
outlet spout to collect the distillate.
5. Make sure all connections fit snugly was checked before the distillation process
begin. The distillation was started by turning on the hot plate. The heating control
switch should be positioned at 6 or 7.
6. When the solution inside the flask is approximately one-third vaporized, the hot
plate was turned off.
7. Wait until the plate cools down and let all the vapours condense before
disassembling the distillation equipment. Should be careful While disassembling
the glassware not to spill any distillate that might be trapped in between the
connections. This trapped distillate should be collect and add up to collecting
beaker
 B. Titration of distillate
1. The collecting beaker was reweighed including its content.
2. All distillate was poured from the beaker into a 250-ml volumetric flask. Wash
onto the flask the remaining distillate left on the beaker-wall with distillate water.
3. Half of the flask was filled with distilled water. Put its cap and shake the flask
gently a few times. Then fill up flask up to the mark with distilled water. Put the
cap on again and the flask was turned upside down a few times so that the solution
is well-mixed.
4. About 100 ml of the diluted solution was poured into a clean beaker. 20 ml or 25
ml of the solution was taken by using a pipette, each into 3 separate clean conical
flasks. Then squeeze 2 drops of phenolphthalein indicator into each flask.
5. A burette was filled with 2.0M NaOH solution and titrate the content of each flask
with NaOH.

C. Titration of liquid residue

1. Steps B1 to B5 was repeated for the liquid residue

RESULTS :
A. Distillation
Residue Distillate
Mass of Mass of Mass of Mass of
empty Erlenmeyer Mass of empty beaker + Mass of
Erlenmeyer flask + residue beaker distillate distillate
flask residue
(g) (g) (g) (g) (g) (g)

112.4342 172.4040 59.7678 62.5388 99.0178 36.479

B. Titration of distillate
Conical flask 1 2 3
Initial reading of NaOH (mL) 50.0 50.0 50.0
Final reading of NaOH (mL) 32.0 32.4 31.8
Volume of NaOH used (mL) 18.0 17.6 18.2

18.0+17.6+18.2
Average volume of NaOH used (mL) =
3
= 17.93 mL
 C. Titration of liquid residue
Conical flask 1 2 3
Initial reading of NaOH (mL) 50.0 50.0 50.0
Final reading of NaOH (mL) 32.2 32.0 31.6
Volume of NaOH used (mL) 17.8 18.0 18.4

17.8+18.0+18.4
Average volume of NaOH used (mL) =
3
= 18.07 mL

QUESTION :
1) Calculate the molar composition of feed solution (Given ρCH3COOH = 1.048
g/mL and ρH2O = 1.000 g/mL)
Answer :
Mass of acetic acid :

MASS(g)
DENSITY =
VOLUME (cm3 )

MASS=DENSITY X VOLUME

Density of acetic acid : 1.048 g / cm3

g
MASS=1.048 3
X 40 cm3
cm

= 41.92 g

SPECIES MASS MOLE (gmol) MOLE MOLE PERCENT

(g) FRACTION (%)
WATER
(A) 10.00 g 0.5556 0.443 x 100%
=0.5556 =0.443
g 1.2543
10.00 18
gmol
= 44.30 %
 ACETIC
ACID 41.92 g 0.6987 0.5570 x 100%
=0.6987 =0.557
g 1.2543
(B) 41.92 60
gmol
= 55.70 %

TOTAL 51.92 1.2543 1.0000 100

2) From titration data, determine the composition of the distillate

Answer :

Acid-base titration :

CH3COOH + NaOH → CH3COONa + H2O

Molarity of NaOH = 2.0 M

Volume of NaOH = 17.93 ml

Molarity of CH3COOH = ?

Volume of CH3COOH = 25 ml

No of mole of CH3COOH = 2.0 (0.01793)

= 0.03586 mol

Since 0.03586 mole of CH3COOH present in 25 ml solution, we need to find the number of
mole of CH3COOH in 250 ml solution which is the composition of the distillate

DILUTION :
M1 V1 = M2 V2
250 ml
X 0.03586 moles of acetic acid ∈25 ml
25 ml
= 0.3586 moles of acetic acid in 250 ml

SPECIES MASS (g) MOLE MOLE MOLE

 MASS
FRACTI FRACTIO PERCENT
(gmol)
ON N (%)

36.479 −¿ 14.963 g 0.6986 x

14.963 0.8313
g
WATER 21.516 36.479 18 1.1899 100%
gmol
(A)
= 14.963 ¿ 0.4102 ¿ 0.6986 = 69.86 %
¿0.8313

21.516 0.3586 0.3014 x

ACETIC 0.3586 x 60
36.479 1.1899 100%
ACID 0.3586
(B) = 21.516
¿ 0.5898 ¿ 0.3014 = 30.14 %

TOTAL 36.479 1.0000 1.1899 1.0000 100

3) From titration data, determine the composition of the residual liquid

Answer :
Acid-base titration :

CH3COOH + NaOH → CH3COONa + H2O

Molarity of NaOH = 2.0 M

Volume of NaOH = 18.07 ml

Molarity or CH3COOH = ?

Volume of CH3COOH = 25 ml

No of mole of CH3COOH = 2.0 (0.01807)

 = 0.03614 mol

Since 0.03614 mole of CH3COOH present in 25 ml solution, we need to find the number of
mole of CH3COOH in 250 ml solution which is the composition of the distillate

DILUTION :
M1 V1 = M2 V2
250 ml
X 0.03614 moles of acetic acid ∈25 ml
25 ml
= 0.3614 moles of acetic acid in 250 ml

MOLE MOLE
MASS MOLE
SPECIES MASS (g) FRACTIO PERCENT
FRACTION (gmol)
N (%)

14.795 g
14.795 0.8219
36.479 – 21.684 g 0.6946 x 100%
WATER 36.479 18 1.1833
gmol
(A)
= 14.795 = 69.46 %
¿0.4056 ¿ 0.6946
¿ 0.8219

21.684 0.3614
ACETIC 0.3614 x 60 0.3054 x 100%
36.479 1.1833
ACID 0.3614
(B) = 21.684 = 30.54 %
¿0.5944 ¿ 0.3054

TOTAL 36.479 1.0000 1.1833 1.0000 100

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

residual liquid. Compare the theoretical values with the experimental values.
(Equilibrium data for water-acetic acid system at 1 atm is provided in
Appendix 1)
 Appendix 1: Equilibrium data for water-acetic acid system at 1 atm

x y
0 0
0.1881 0.3063
0.3084 0.4487
0.4498 0.5973
0.5195 0.658
0.5824 0.7112
0.675 0.7797
0.7951 0.8671
0.8556 0.9042
0.8787 0.9185
0.9134 0.9409
0.9578 0.9708
1 1

5) What is the advantages of batch distillation compare with simple equilibrium

distillation?
Answer :
 In batch distillation, feed quantity small than simple equilibrium distillation. It
relatively small quantities of material are to be handled at regularly scheduled periods.
Batch distillation also economial for small volumes productions.
 Batch distillation is flexibility. Its little change is required when switching from one
mixture to another. It is flexible in accommodating changes in product formulation,
changes in production, changes in feed composition and the others