1.

0 Results and Discussion

Time Temperature Readings ( º C ) RI RI

(Min) TI 1 TI TI TI 2 TI TI TI 4 TI 5 TI6 Top Bottom
1A 1B 2A 2B Product Product
0 34 82 90 95 94 97 94 28 32 1.353 1.335
5 34 86 90 96 94 97 94 30 32 1.351 1.335
10 34 87 92 97 96 98 96 28 33 1.350 1.334
15 34 89 92 98 96 99 96 29 33 1.350 1.334
20 35 89 93 98 97 99 96 29 33 1.349 1.335
25 34 89 94 97 97 100 97 29 33 1.348 1.335
30 34 89 94 99 97 100 97 29 33 1.349 1.335
35 34 89 95 99 97 100 97 29 33 1.350 1.335
40 35 89 95 100 98 100 97 29 33 1.349 1.333
45 34 89 95 100 98 101 98 29 33 1.348 1.333
50 34 89 96 100 99 101 98 29 33 1.347 1.333
55 34 89 96 101 99 101 98 29 33 1.347 1.333
60 34 89 96 101 99 101 98 29 33 1.347 1.333

Table 1: Readings from experiment

Time (min) RI Top Product Concentration RI Bottom Concentration

of Product of Ethanol
Ethanol(%w/w) (%w/w) Bottom
Top Product Product
0 1.353 28.00 1.335 4.00
5 1.351 26.00 1.335 4.00
10 1.350 24.00 1.334 2.00
15 1.350 24.00 1.334 2.00
20 1.349 23.00 1.335 4.00
25 1.348 22.00 1.335 4.00
30 1.349 23.00 1.335 4.00
35 1.350 24.00 1.335 4.00
40 1.349 23.00 1.333 0.00
45 1.348 22.00 1.333 0.00
50 1.347 20.00 1.333 0.00
55 1.347 20.00 1.333 0.00
60 1.347 20.00 1.333 0.00
Table 2: Concentration of ethanol (%w/w)
 In this experiment, the Bubble Cap distillation column was conducted to mass
balance from operate vapour liquid separation using Bubble Packed Column Distillation
Unit. From the result its shows the the longer the time taken, the higher the temperature
thus, the value refractive index of the component was closed to the original value refractive
index of water (1.33) and ethanol (1.361). This is because the time taken during this
experiment is only 60 min. For this type of distillation it takes several hours to separate the
compounds. From the result we can obtained the concentration of methanol at top and
bottom product. The concentration of ethanol at top product constant at 50 min which is
20.00 %w/w, while the bottom product the concentration ethanol starting to constant at 40.00
%w/w with 0.0 %w/w. By conducting the mass balance, the mass of feed that goes into the
process is 29. 5505 kg. While the output at top is = 4.438 kg while the bottom is 25.1123 kg.

Mole Fraction of Ethanol vs RI Top Product

0.3
Mole Fraction of Ethanol

0.25
0.2
0.15
0.1
0.05
0
1.346 1.347 1.348 1.349 1.35 1.351 1.352 1.353 1.354
Refractive Index

Graph 1
 Mole Fraction of Ethanol vs RI Bottom
Product
0.05

Mole Fraction of Ethanol

0.04

0.03

0.02

0.01

0
1.3325 1.333 1.3335 1.334 1.3345 1.335 1.3355
-0.01
Refractive Index

Graph 2
From the value of Refractive Index for ethanol, the concentration of ethanol (%w/w) can be
obtained. For the calculation of mass balance, the final constant value of the Refractive
Index is used. By referring to Appendix A,
For nethanol = 1.347, the concentration (%w/w) is approximately 20 %w/w.
Mass balance for this process in done to calculate the unknown values.
It is known that the Feed contains 25 L water, Ethanol with 90%w/w.

P1 =? Kg

Ethanol, C2H6O
20 %w/w

Separator

Feed=? Kg
25 L H2O
5 L C2H6O
 90%w/w C2H6O
P2 =? Kg

Water, H2O
100 %w/w
Since Feed is in unit Litres, convert into unit kg to perform the mass balance.
𝑔 𝑔 𝑔 𝑘𝑔
𝑀𝑤H2O = 18.016 , 𝑀𝑤C2H6O = 46.068 , 𝜌H2O = 1 3 , 𝜌C2H6O = 789 3
𝑚𝑜𝑙 𝑚𝑜𝑙 𝑐𝑚 𝑚

For 25 L H2O,
1 𝑐𝑚3 1𝑔
25 L H2O. 1𝑥10−3 𝐿
. 1 𝑐𝑚3

= 25 000 g H2O
= 25 kg H2O
For 5 L of 90% C2H6O, the mass of H2O is
10 H2O 1 𝑐𝑚3 1𝑔
5 L total. 100 total
. 1𝑥10−3 𝐿
. 1 𝑐𝑚3

= 500 g H2O
= 0.5 kg H2O
For 5 L of 90% C2H6O, the mass of C2H6O is
90 C2H6O 1 𝑐𝑚3 1𝑥10−6 𝑚3 789 𝑘𝑔
5 L total. . . .
100 total 1𝑥10−3 𝐿 1𝑐𝑚3 𝑚3

= 3.5505 kg C2H6O
Thus, total Feed in kg is
Feed = 25 kg H2O + 0.5 kg H2O + 3.5505 kg C2H6O
= 29. 5505 kg

Calculation to find the unknowns in the systems.

Degree of Freedom

 2 Unknowns : P1 , P2
 2 Equations : Overall mass balance, Ethanol mass balance

Ethanol Mass Balance

3.5505 kg = P1 (0.8)
P1 = 4.438 kg
Overall Mass Balance
Feed = P1 + P2
29.5505 kg = 4.438 kg + P2
P2 = 25.1123 kg
 In distillation bubble cap process, usually a part of the condensed overhead product
is returned back to the top column which is known as reflux. (Muhammad , 2015). The reflux
ratio is the ratio between the boil up rate and the take-off rate. It is the ratio between the
amount of reflux that goes back down the distillation process and the amount of reflux that is
collected in the distilation to produce again product and waste. The higher the reflux ratio,
the more vapour/liquid contact can occur the distillation column. So higher the reflux ratio
usually means higher purity of distillate. In this experiment we only used 1.0 so the
concentration of ethanol at top product are 20.00 %w/w and the concentration of ethanol at
bottom product is 0.00. if the reflux ratio is higher, the possibility to gain purity of water and
ethanol are higher.
5.0 Appendix

Refractive indices of ethanol solutions at 20 °C, 589.29 nm

concentration
n
% w/w
0.00 1.3330 34.00 1.3557 68.00 1.3650

2.00 1.3342 36.00 1.3566 70.00 1.3652

4.00 1.3354 38.00 1.3575 72.00 1.3654

6.00 1.3367 40.00 1.3583 74.00 1.3655

8.00 1.3381 42.00 1.3590 76.00 1.3657

10.00 1.3395 44.00 1.3598 78.00 1.3657

12.00 1.3410 46.00 1.3604 80.00 1.3658

14.00 1.3425 48.00 1.3610 82.00 1.3657

16.00 1.3440 50.00 1.3616 84.00 1.3656

18.00 1.3455 52.00 1.3621 86.00 1.3655

20.00 1.3469 54.00 1.3626 88.00 1.3653

22.00 1.3484 56.00 1.3630 90.00 1.3650

24.00 1.3498 58.00 1.3634 92.00 1.3646

26.00 1.3511 60.00 1.3638 94.00 1.3642

28.00 1.3524 62.00 1.3641 96.00 1.3636

30.00 1.3535 64.00 1.3644 98.00 1.3630

32.00 1.3546 66.00 1.3647 100.00 1.3614

Table of contents

Content Page Number

Summary

1.0 Results and Discussion

2.0 Conclusions and Recommendations

3.0 Tutorial

4.0 References

5.0 Appendices
3.0 Tutorial

1. Describe an example of industrial applications that utilized distillation in its process.

Discuss the advantages and disadvantages of using bubble cap distillation process in
chemical plant.

 The example of industrial applications that utilized distillation in its process,the

process of reactive distillation involves using the reaction vessel as the still. In this
process, the product is usually significantly lower-boiling than its reactants. As the
product is formed from the reactants, it is vaporized and removed from the reaction
mixture.The advantages of using bubble cap distillation process are the liquid/vapor
contact in the cross-flow of plate columns is more effective than the countercurrent-
flow in packed columns and can handle high liquid flow rates cost-effectively.The
disadvantages of using bubble cap distillation process are higher pressure drops
than packed columns which could cause column flooding and foaming can occur due
to agitation of the liquid by the vapor flowing up through it.

2. Write a one paragraph summary of any journal article that studies distillation
process.The article must been published within the last 5 years.Explain on the
distillation process type used in the study and its significance to study done.

 Experimental data and simulations in Aspen Plus® for the batch distillation process
were obtained from an ethanol/water mixture. The simulation was carried out in order
to verify the effectiveness of the calculations for the batch distillation process for
recovering ethanol, using a plate column. The experimental data were taken from a
packed batch distillation column. The separation of ethanol/water mixture was
studied at different reflux ratios. The ethanol was quantified through a gas
chromatography analyses. The simulation and the experimental data were performed
considering the ethanol concentration in the wine that comes from the sugarcane
fermentation. It was verified that the higher ethanol concentration was obtained in
one hour of distillation and the accumulate ethanol concentration was above to 80%
(mole) when operated at constant reflux. So, it is possible to obtain high yields and
concentrations of ethanol in a short time.
4.0 Preferences

1. Bravo, Jose L. and James K. Fair. "Distillation Columns." Chemical Engineering

Progress January 1990:19-29.

2. Distillation Columns, 2017, University of Michigan, [Online]. [ Accessed on 25TH

Sept,2017] Available from world wide website :
http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationColu
mns/DistillationColumns.html

3. Jenkins, John and Ken Porter. "Distillation Now." The Chemical Engineer November
1985: 26-30.

4. M.E.TAlvareza, E.B.Moraesa, J.C.Rodriguesab, A.J.Bonona, M.R.Wolf-Maciela.

“Evaluation of the batch distillation process in the ethanol production”. Computer
Aided Chemical Engineering 2012 : 632-636

5. Refractometer.pI. (2011). Refractive index of ethanol solutions. Retrieved from

http://www.refractometer.pl/refraction-datasheet-ethanol

6. Muhammad Rashid Usman (2015). Comprehensive Dictionary of Chemical

Engineering. Pakistan: Lulu.

7. Williamson, K & Masters, K. (2011). Techniques Labs for Macroscale and Microscale
Organic Experiments, United Kingdom: Mary Fich.

8. Sirkar, Kamalesh K. (2014). Separation Of Molecules, Macromolecules And Particles:

Principles, Phenomena And Processes. Cambridge, [England]: Cambridge University
Press
Summary
Objectives of the experiment is to separate a mixture of two miscible liquids (liquids that mix
in all proportions) with different boiling points. It will accomplish this by a separation
procedure known as distillation, which relies on each compound having a distinct and
separate boiling point. Then it also to conduct mass balance and energy balance in
distillation process to compare the experimental results and predict the results from
software. Based on the data, in minute 45 the temperature reading (oc) start constant. The
top product reading constant at 1.348 and the concentration of ethanol (% w/w) is 22.00
while the lower product reading is 1.333 and the concentration of ethanol (% w/w) is 0.00.
The graft is same as in the laboratory manual. This experiment that have been carried out
were successful with the objectives of this experiment is to separate two volatile compounds
from a mixture due to the different chemical properties of each compound. Which is it is a
physical process used to separate chemicals from a mixture by the difference in how easily
they vaporize. As the mixture is heated, the temperature rises until it reaches the
temperature of the lowest boiling substance in the mixture, while the other components of
the mixture remain in their original phase in the mixture. This experiment runs smoothly
based on method given and data have been collected during experiment which is the graph
from the experiment result is same as in the laboratory manual.
2.0 Conclusion and recommendation
As a conclusion,this experiment that have been carried out were successful. The objectives
of this experiment is to separate two volatile compounds from a mixture due to the different
chemical properties of each compound. It will accomplish this by a separation procedure
known as distillation, which relies on each compound having a distinct and separate boiling
point. It is a physical process used to separate chemicals from a mixture by the difference in
how easily they vaporize. As the mixture is heated, the temperature rises until it reaches the
temperature of the lowest boiling substance in the mixture, while the other components of
the mixture remain in their original phase in the mixture. The resultant hot vapor passes into
a condenser and is converted to the liquid, which is then collected in a receiver flask. The
other components of the mixture remain in their original phase until the most volatile
substance has all boiled off. Only then does the temperature of the gas phase rises again
until it reaches the boiling point of a second component in the mixture, and so on. This
experiment runs smoothly based on method given and data have been collected during
experiment which is the graph from the experiment result is same as in the laboratory
manual.
The recommendation in apparatus is provide a small size of rubber glove such as S size
because the XL size glove in the laboratory makes it difficult for students to undergo
experiments due to small hand sizes.