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CMT267 - Simple Batch Distillation

This experiment aimed to separate a mixture of acetic acid and water using distillation. The mixture was heated to vaporize it, then the vapors were condensed to obtain separate distillate and residue liquids. Titrations of the distillate and residue using NaOH determined the composition of each. Calculations were done to find the molar composition of the original feed solution based on the measured masses and densities of acetic acid and water used.
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0% found this document useful (0 votes)
108 views

CMT267 - Simple Batch Distillation

This experiment aimed to separate a mixture of acetic acid and water using distillation. The mixture was heated to vaporize it, then the vapors were condensed to obtain separate distillate and residue liquids. Titrations of the distillate and residue using NaOH determined the composition of each. Calculations were done to find the molar composition of the original feed solution based on the measured masses and densities of acetic acid and water used.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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ABSTRACT

This experiment was conducted to separate an ordinary binary mixture consisting of


acetic acid and water using a simple batch distillation technique and to determine the
composition of distillate and residual liquid. It was aimed to separate a mixture of liquids by
distillation, the liquid can be heated to force components to turn it into vapor phase. Binary liquid
consists of two different liquids , thus it has different capability to change phases to vapours.

To start the experiment, in distillation at A section, we prepared an acetic acid-water


solution by adding 40 mL acetic acid to 20 mL distilled water in an Erlenmeyer flask. In terms of
heating, we put the flask on a hot plate . Then, the tap was turned on gently to let cooling water
into the condenser. Also, the clean beaker was positioned beneath to collect the distillate. The
hot plate was turned off when the solution was one third vaporized. We have been waiting to let
the plate cool down in order to let all the vapors condensed.

Then, in this experiment , we also did two titrations which were titration of distillate and
titration of residual. We poured the content which was distillate and the residue into different 250
mL of volumetric flask. Then we filled half of the flask with distilled water. We shook it gently and
then filled up the flask to the mark with distilled water. After shaking to mix well, we poured
about 100 mL dilution solution from each of them to pipette with 2.0 M NaOH solution in a
conical flask. Then the end point was seen by the colour changes using phenolphthalein as
indicator.
INTRODUCTION

Distillation is used for separating mixture based on difference in boiling point. The
earliest method of separation and the most common unit activity in industry is distillation. It
involves separating a mixture based on the volatility or boiling point of its main components.
Distillation is used to separate a mixture of liquids, the liquid can be heated to force components
to turn into vapor phase. Also, it is a procedure where a liquid sample is volatilized to create a
vapor, which is then condensed to obtain a liquid that is richer in the more volatile components
of the original sample. The process of evaporation normally involves heating the liquid, however
it can also be accomplished by lowering the pressure or by combining the two processes.
Furthermore, the gas that is produced is then condensed back into liquid form and collected is
called distillate. Distillate is the vapour from a distillation that is trapped and condensed into a
liquid known as a distillate. It can also be the name of the substance that results during
distillation. In addition, the original mixture contains less volatile compounds called residues.

The physical concept of distillation is evaporation, it consists of the process of phase


transformation from liquid phase to gas phase or vapor phase. On behalf of that, volatility is
considered too , where it possesses the tendency of liquid to change form to gas. Regarding the
evaporation process, molecules of liquids are held close by intermolecular forces which are
hydrogen bonding and van der waal. Because intermolecular forces must be overcome,
molecules that are forced apart become weaker. Thus, molecular separation needs energy and
is supplied by surrounding or external heating which impacts the intermolecular forces to be
broken, so more vapour is produced per unit time.

In terms of binary mixture, it consists of two different phases, for example, acetic acid
and water. Also, different liquids have different capability to change phases to vapours. Binary
liquid mixes are liquids made up of A and B, two different kinds of molecules. A common binary
liquid mixture will phase separate into two different liquid phases for a certain range of
temperatures and concentrations, similar to acetic acid and water mix. Thus, binary solutions
also include two components that are combined uniformly and in a homogenous form. But the
solvent might be a gas or a liquid.
OBJECTIVES

1. To separate an ordinary binary mixture consisting of acetic acid and water using a simple
batch distillation technique.

2. To determine the composition of distillate and residual liquid.

APPARATUS AND CHEMICAL

Beaker, 250 mL volumetric flask, Burette with clamp pipette, Suction bulb, Heating mantle,
Conical flask , Distilling head, Thermometer with adapter, Retort Stand with clamp, Dropper,
Condenser, Acetic acid, Distilled water, 2.0 M NaOH, and Phenolphthalein
PROCEDURE

A. Distillation

1. An acetic acid-water distillation was prepared by adding 40mL acetic acid to 20mL
distilled water in an Erlenmeyer flask.
2. The flask was put on a hot plate. The solution was prepared for distillation using
equipment from the distillation kit, as demonstrated by the instructor.
3. To introduce cooling water into the condenser, the tap was gradually opened. The hose
for the outlet water was made sure to be inside the sink. The inlet was adjusted so that
the cooling water entered at a rate sufficiently high enough to cool and vapour was
condensed completely.
4. A clean and dry 150 mL beaker was weighted and was positioned beneath the distillate
outlet spout to collect the distillate.
5. All the connection was checked to make sure that it fits snugly before the process
begins. The distillation was started by turning on the hot plate. The heating control switch
is positioned at 6 or 7.
6. The hot place was turned off when the solution inside the flask was approximately
one-third vaporized.
7. The plate cools down to let all vapours condense before disassembling the distillation
equipment. The trapped distillate was collected and added up to the collecting beaker.

B. Titration of distillate

1. The collecting beaker was reweighted including its contents.


2. All the distillate from the beaker was poured into a 250 mL volumetric flask. The flask
was washed onto the remaining distillate left on the beaker wall with distilled water.
3. Half of the flask was filled with distilled water. The cap was put on and the flask shaked
gently a few times. It was then filled up to the mark with distilled water. The cap was put
again and turned the flask upside down a few times so that the solution is well mixed.
4. About 100 mL of diluted solution was poured into a clean beaker. 20 mL of the solution
was taken using pipette into 3 separate clean conical flasks. Then, two drops of
phenolphthalein indicator were added into each flask.
5. The burette was filled with 2.0 M NaOH solution and titrated the content of each flask
with naOH.
C. Titration of liquid residue

1. The collecting beaker was reweighted including its contents.


2. All the residue from the beaker was poured into a 250 mL volumetric flask. The flask was
washed onto the remaining residue left on the beaker wall with distilled water.
3. Half of the flask was filled with distilled water. The cap was put on and the flask shaked
gently a few times. It was then filled up to the mark with distilled water. The cap was put
again and turned the flask upside down a few times so that the solution is well mixed.
4. About 100 mL of diluted solution was poured into a clean beaker. 20 mL of the solution
was taken using pipette into 3 separate clean conical flasks. Then, two drops of
phenolphthalein indicator were added into each flask.
5. The burette was filled with 2.0 M NaOH solution and titrated the content of each flask
with NaOH.

RESULT AND CALCULATION

A. Distillation

RESIDUE DISTILLATE

Mass of Mass of Mass of Mass of Mass of Mass of


empty beaker + residue (g) empty beaker beaker + distillate
beaker (g) residue (g) (g) distillate (g)

62 98.30 36.30 62 81.66 19.66

B. Titration of distillate

Erlenmeyer flask 1 2 3
Initial reading of 0 10 19.9
NaOH (mL)

Final reading of 10 19.9 29.5


NaOH (mL)

Volume of NaOH 10 9.9 9.6


(mL)

Average of NaOH 9.83


used (mL)

C. Titration of residue

Erlenmeyer flask 1 2 3

Initial reading of 0 21.6 0


NaOH (mL)

Final reading of 21.60 43.6 22


NaOH (mL)

Volume of NaOH 21.60 22 22


(mL)

Average of NaOH 21.87


used (mL)

CALCULATION

a) Distillation

Residue = 98.30 – 62

= 36.30 g

Distillate = 81.66 – 62

= 19.66 g
b) Titration of Distillate

10 + 9.9 + 9.6
Average volume of NaOH used = 3

= 9.83 mL

c) Titration of liquid Residue

21.60 + 22 + 22
Average volume of NaOH used = 3

= 21.87 mL
DISCUSSION
QUESTIONS

1 .Calculate the molar composition of feed solution ( Given density CH3COOH = 1.048
g/mL and density H2O = 1.000 g/mL)

The mass of acetic acid and water.

Mass= Density x Volume

Masswater = 1.000 g/mL x 20 mL

= 20 g

Massacetic acid = 1.048 g/mL x 40 mL

= 41.92 g

Mole of acetic acid and water.

𝑀𝑎𝑠𝑠
Mole =
𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠

20 𝑔
Molewater = 18.02 𝑔/𝑚𝑜𝑙

= 1.11 mol

41.92 𝑔
Moleacetic acid = 60.05 𝑔/𝑚𝑜𝑙

= 0.698 mol
Mole fraction of acetic acid and water

𝑀𝑜𝑙𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝐴
Mole fraction =
𝑀𝑜𝑙𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝐴+ 𝐵

1.11 𝑚𝑜𝑙
Mole fractionwater = 1.11 𝑚𝑜𝑙 + 0.698 𝑚𝑜𝑙

= 0.614

0.698 𝑚𝑜𝑙
Mole fractionacetic acid = 1.11 𝑚𝑜𝑙 + 0.698 𝑚𝑜𝑙

= 0.386

Percentage of acetic acid and water

Percentage of each component = mole fraction x 100 %

Percentagewater = 0.614 x 100 %

= 61.4 %

Percentageacetic acid = 0.386 x 100 %

= 38.6 %

Component Mass (g) Mole (mol) Mole fraction Mole fraction


Percentage (%)

Water 20.00 g 1.110 mol 0.614 61.40 %

Acetic acid 41.92 g 0.698 mol 0.386 38.60 %


Total 61.92 g 1.808 mol 1.000 100 %

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

CH3COOH + NaOH → CH3COONa + H2O

No. of moles NaOH = MV/1000

= (2.0)(9.83)/1000

= 0.01966 moles

1 mole of NaOH react with 1 mole of CH3COOH

No. of moles CH3COOH = 0.01966 moles

0.01966 moles of CH3COOH are present in 25 mL

No. of moles of CH3COOH present in 250 mL = 250 (0.01966) / 20

= 0.2456 moles

Composition Mass (g) Mass Mole (g/mol) Mole Fraction Mole


Fraction precent

Water (A) 19.66 g – 4.924/19.66 4.924/18 0.2736/0.5190 0.5272 x


0.2456 g 100 %
=0.2505 =0.2736 =0.5272
=4.924 g
=52.72 %
Acetic Acid 0.2456 14.736/19.66 14.736/60.05 0.2454/0.5190 0.4728 x
(B) mol x 60 100 %
g/mol =0.7495 =0.2454 =0.4728
=47.28 %
=14.736 g

Total 19.66 g 1.0000 0.5190 1.0000 100

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

CH3COOH + NaOH → CH3COONa + H2O

No. of moles NaOH = MV/1000

= (2.0)(21.87)/1000

= 0.04362 moles

1 mole of NaOH react with 1 mole of CH3COOH

No. of moles CH3COOH present in 25 mL = 0.04362 moles

No. of moles of CH3COOH in 250 mL = 250 (0.04362) / 20

= 0.5453 moles

Composition Mass (g) Mass Mole Mole Fraction Mole


Fraction (g/mol) precent
Water (A) 36.30 g – 3.582/36.30 3.582/18 0.1990/0.7438 0.2675 x
32.718 g 100 %
=0.0987 =0.1990 =0.2675
=3.582 g
26.75%

Acetic Acid 0.5453 32.718/36.30 32.718/60.0 0.5448/0.7438 0.7325 x


(B) mol x 60 5 100 %
g/mol =0.9013 =0.7325
=0.5448 =73.25 %
=32.718 g

Total 36.30 g 1.0000 0.7438 1.0000 100


CONCLUSION

In conclusion the objective of this experiment were achieved.We managed to separate an


ordinary binary mixture consisting of acetic acid and water using a simple batch distillation
technique.Also,the composition of distillate and residual liquid can be determined.Based of the
data that we recorded,the mass for both residue and distillate are 36.30 g and 19.66 g.Next,the
average of NaOH that be used in the titration for distillate is 9.83 mL while for residue is
21.87.Lastly,the percentage of each composition which are water and acetic acid in the distillate
is 52.72% and 47.28 %.Meanwhile the percentage of water and acetic acid that contains in
residual is 26.75 % and 73.25% respectively.
REFERENCES
Anne Marie Helmenstine , (5 September , 2019) , Distillate Definition in Chemistry , Retrieved
15 January , 2023 from https://www.thoughtco.com/definition-of-distillate-604718
Levente Cseri , (2018) , Organic Solvents in Sustainable Synthesis and Engineering , Retrieved
15 January , 2023 from
https://www.sciencedirect.com/topics/earth-and-planetary-sciences/distillation

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