FACULTY OF CHEMICAL ENGINEERING

Universiti Teknologi MARA

Cawangan Sarawak
Kampus Samarahan
94300 Kota Samarahan, SARAWAK
Tel : +6082-677200 Fax: +6082-677300

TECHNICAL REPORT :
CHE249 SEPARATION PROCESSES

Lab Title : M2 - Distillation Column Experiment

100
Semester : MARCH – AUGUST 2022 Date Performed : 25th April 2022
Group members
*Please cancel which is not
Group: EH110-4B
necessary. No. Name UiTM Student No. Signature
1 INTAN NURSYAHIRAH BINTI MOHD NADZRI 2020868634
2 NUR AMIRAH BINTI MOHD AMEZAN 2020815928
3 NURUL IFFAH BINTI FISAL 2020893314

4 NURIN SYAZA SYAFIQAH BINTI SHAHRUL 2020463664

NIZAM

CRITERIA FULL MARKS MARKS

Part 1: Practical Demonstration
Practical Demonstration on 20
- Operating Procedures (Start-Up Procedures and
Shut-Down Procedures)
- Experiment Procedures
- Sampling Procedures
Part 2: Technical Report
Data/Results/Calculation
• Technical 20

• Non - Technical 10

Discussion 25

Conclusion 10

Appendices /References 5

Timelines 5

Organization & Appearance 5

TOTAL MARKS 100

Remarks:
Summar Distillation is a method of purifying liquids by which the components of a
y of mixture can be separated when their boiling points are considerably different. A
Theory liquid is boiled in a "distilling flask, then the vapours flow into another part of the
apparatus and come into contact with a cool surface. The vapours condense on the
cool surface and the condensed liquid (distillate) drips into a reservoir separate from
the original liquid.
When a liquid mixture is heated to boiling point, the vapour above the liquid
has a different composition than the liquid. When this vapour is separated and
condensed to a liquid, the lower boiling component(s) of the original combination
become richer, as shown in Figure 1.

The distillation column was set to total reflux. Total reflux is a condition where
vapour and liquid flow through the column, but no product is removed. The slopes
of the operating lines are then L/V = 1.0, which means in terms of mass balance, that
each plate is y = x. The number of plates theoretically required is minimal at 100%
reflux. The number of plates needed increases when the reflux ratio is reduced by
removing the product. The separation process can therefore be carried out at any
reflux ratio above the minimum reflux ratio.
The bubble curve is the first vapour bubble formed when a subcooled liquid is
heated. The dew curve is the first drop of liquid formed when a superheated vapour
is cooled.
𝑥 = 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑚. 𝑣. 𝑐 𝑖𝑛 𝑙𝑖𝑞𝑢𝑖𝑑
𝑦 = 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑚. 𝑣. 𝑐 𝑖𝑛 𝑣𝑎𝑝𝑜𝑢𝑟

In simplest terms, distillation is a process in which two phases, liquid, and

vapour, are in equilibrium. In a pure compound, especially a pure ionic compound,
there is often a high boiling point. However, in a mixture, there is phase equilibrium
over a range of temperatures. The temperature-composition diagram for an isobaric
condition is shown in Figure 2.
 All in all, the separation of a mixture by distillation is determined by the
difference in the composition of a boiling liquid mixture and the vapour mixture at
equilibrium. Since ethanol is more volatile than water in this experiment, it has a
higher vapour pressure at the same temperature. As a result, y is greater than x at
equilibrium. A distillation column with a boiler at the bottom and a condenser at the
top allows contact between rising vapour and descending liquid in countercurrent.
As a result, the ethanol accumulates at the top of the column while the water
accumulates at the bottom.

Data/
Result/ Table 1 Calibration Data

Graph Amount of Amount of Ethanol Composition Refractive

ethanol water Index (RI)
Vol% Mol%
(mL) (mL)

0 100 0.0 0.00 1.3281

10 90 10.0 3.31 1.3325

20 80 20.0 7.16 1.3385

30 70 30.0 11.68 1.3436

40 60 40.0 17.06 1.3483

50 50 50.0 23.58 1.3520

60 40 60.0 31.64 1.3539

 70 30 70.0 41.86 1.3561

80 20 80.0 55.25 1.3568

90 10 90.0 73.53 1.3569

100 0 100.0 100.00 1.3570

Table 2 Properties of Pure Components

Ethanol, 𝑪𝟐 𝑯𝟓 𝑶𝑯 Water, 𝑯𝟐 𝑶
Density (𝒈⁄𝒎𝑳) 0.789 1.00
Molecular Weight 46.07 18.02
(𝒈⁄𝒎𝒐𝒍)

Table 3 Result

Tray Refractive Index, RI Mol fraction (Ethanol)

(nD)
Distillate 1.3408 0.40
Feed 1.3330 0.21
Bottom 1.3323 0.19

Table 4 Mol Fraction (%) of Ethanol

Ethanol, 𝑪𝟐 𝑯𝟓 𝑶𝑯 Water, 𝑯𝟐 𝑶 (mole) Mol Fraction (Ethanol)

(mole)
0.0000 5.5494 0.0000
0.1712 4.9945 0.0331
0.3425 4.4395 0.0716
0.5138 3.8846 0.1168
0.6851 3.3296 0.1706
0.8563 2.7747 0.2358
1.0276 2.2198 0.3164
1.1988 1.6648 0.4186
1.3701 1.1099 0.5525
1.5414 0.5549 0.7353
1.7126 0.0000 1.0000

Table 5 Summary of Moles fraction and Mass Fraction of Ethanol

Moles of Moles of Mole Mass of Mass of Mass
Ethanol Water Fraction of Ethanol Water Fraction of
Ethanol Ethanol
0.0000 5.5494 0.0000 0.00 100 0.0000
0.1713 4.9945 0.0331 7.89 90 0.0806
0.3425 4.4395 0.0716 15.78 80 0.1648
0.5138 3.8846 0.1168 23.67 70 0.2527
0.6851 3.3296 0.1706 31.56 60 0.3447
0.8563 2.7747 0.2358 39.45 50 0.4410
1.0276 2.2198 0.3164 47.34 40 0.5420
1.1988 1.6648 0.4186 55.23 30 0.6480
1.3701 1.1099 0.5525 63.12 20 0.7594
1.5414 0.5549 0.7353 71.01 10 0.8766
1.7126 0.0000 1.0000 78.90 0 1.0000

Table 6 Calculation Formulae

𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙
1
= 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑚𝐿) × 𝑔
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 ( )
𝑚𝑜𝑙
𝑔
× 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 ( )
𝑚𝐿
1 𝑔
= 10 (𝑚𝐿) × 𝑔 × 0.789
46.07 𝑚𝐿
𝑚𝐿

= 0.1713𝑔

1
𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 = 𝑤𝑎𝑡𝑒𝑟 (𝑚𝐿) ×
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑔/𝑚𝑜𝑙)
× 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑔/𝑚𝐿)
𝑔 1
= 90 (𝑚𝐿) × 0.997 × 𝑔
𝑚𝐿 18.02
𝑚𝐿

= 4.9795 𝑔/𝑚𝐿

𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙
𝑀𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 =
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 + 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
0.1713𝑔
=
0.1713𝑔 + 4.9795𝑔
= 0.333 𝑔/𝑚𝐿
 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙
𝑀𝑜𝑙 % 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 = × 100%
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 + 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
0.1713𝑔
= × 100%
0.1713𝑔 + 4.9795𝑔
= 3.33 𝑚𝑜𝑙%
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑚𝐿)
𝑉𝑜𝑙 % 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 = × 100%
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑚𝐿) + 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑚𝐿)
10 (𝑚𝐿)
= × 100%
10 (𝑚𝐿) + 90 (𝑚𝐿)
10 (𝑚𝐿)
= × 100%
100 (𝑚𝐿)
= 10%
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 = 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔⁄𝑚𝐿) × 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑚𝐿)
𝑔
= 0.789 × 90 (𝑚𝐿)
𝑚𝐿
= 71.01 (𝑔)
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑊𝑎𝑡𝑒𝑟 = 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑔⁄𝑚𝐿) × 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑚𝐿)
= 0.997 (𝑔⁄𝑚𝐿) × 90 (𝑚𝐿)
= 89.73 𝑔
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔)
𝑀𝑎𝑠𝑠 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 =
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔) + 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑔)
71.01(𝑔)
=
71.01 (𝑔) + 89.73 (𝑔)

71.01(𝑔)
=
160.74 (𝑔)
= 0.4417
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔)
𝑊𝑡 % 𝑜𝑓 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 = × 100%
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 (𝑔) + 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 (𝑔)
71.01(𝑔)
= × 100%
71.01 (𝑔) + 89.73 (𝑔)
71.01(𝑔)
= × 100%
160.74 (𝑔)
= 44.1769
 Calibration Graph
Graph 1: Refractive Index versus Mole Fraction of Ethanol

Refravtive Index vs Mole Fraction of Ethanol

1.36

1.355

1.35
Refractive Index

1.345

1.34

1.335

1.33

1.325
0 0.2 0.4 0.6 0.8 1 1.2
Mole Fraction of Ethanol

X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm

Graph 2 Mole Fraction of Ethanol versus Mass Fraction of Ethanol

Discussi In a trayed distillation column, each stage is essentially a flash drum, where
vapor from below meets liquid from above. The phases should ideally mix, reach
on
equilibrium, and then separate. The tower is just a practical way of arranging many
mixing stages and efficiently handling internal recycles (boil-up and reflux). The
number of actual stages is displayed on the picture by the number of steps, which is
the same as the number of trays found on the distillation column, based on this
experiment. In the chemical process sector, distillation columns are the major
 equipment used to separate organic compounds involving two or more distinct
components. In most cases, the distillation tower is not self-contained. This is
because distillation columns are frequently connected to both upstream and
downstream equipment. Together, they form a whole process system. As a result,
the better the distillation column works, the better the entire system performs.

Inefficiencies, bottlenecks, and sudden shutdowns are likely to be the most

common issues we'll face with columns. Aside from that, most issues that arise when
doing a distillation column lab experiment are caused by factors that affect the
distillation column's operation. Feed conditions, internal liquid, and fluid flow
conditions, and the state of the machine are all elements to considerate conditions
and trays new advancements in column internals are being investigated, and present
technologies are being upgraded, to help optimize their performance and keep units
working longer. As a result, not only is mass transfer performance more reliable, but
it is also more cost-effective. The status of the trays and packing has the most impact
on the experiment that we do. The efficiency of the plate determines the actual
number of trays required for a given separation task. The elements that induce a drop
in tray efficiency will also affect the column's performance. As a result, more
specific materials for tray construction should be specified. The fundamental
purpose of tray efficiency is to assess a tray's performance. Distillation trays are used
to test theoretical performance against the theoretical maximum.

Conclus In conclusion, this experiment has not achieved their objective which was to
ion determine the number of theoretical plates at total reflux. From the experiment, the
McCabe-Thiele method are used to determine the number of theoretical plates. The
result that we get is 0 which is means the efficiency of the separation process is very
low. This may be due to some error that occur during the experiment. For example,
inefficiencies, bottlenecks, and sudden shutdowns are likely to be the most common
issues we'll face with columns.

Referen
1) Summary. Neutrium. (n.d.). Retrieved May 27, 2022, from
ce https://neutrium.net/equipment/distillation-tray-efficiency/
2) Syahiirah, N. (2018, May 18). CHE504 - Lab Report on distillation column
(L6) (2018). Academia.edu. Retrieved May 27, 2022, from
https://www.academia.edu/36667641/CHE504_Lab_Report_on_Distillatio
n_Column_L6_2018_
3) Wikimedia Foundation. (2022, January 5). Theoretical plate. Wikipedia.
Retrieved May 27, 2022, from
https://en.wikipedia.org/wiki/Theoretical_plate