LABORATORY REPORT

UNIT OPERATION PRACTICAL 2

MODULE: DISTILLATION

Written By:
Group 7 (Thursday)
Widyapradnya Paramita 1706020755
Raissa Samara Natalia Siregar 1706020004
Muhammad Raihan Suprajeni 1706063943

CHEMICAL ENGINEERING DEPARTMENT

ENGINEERING FACULTY
UNIVERSITAS INDONESIA
DEPOK 2020

 TABLE OF CONTENTS

CHAPTER I INTRODUCTION ......................................................................................................... 4

1.1. Experiment Objectives ........................................................................................................ 4
1.2. Basic Theory ........................................................................................................................ 4

CHAPTER II EXPERIMENT AND OBSERVATION DATA ...................................................... 11

2.1. Equipment and Materials ................................................................................................. 11
2.1.1. Equipment ................................................................................................................. 11
2.1.2. Materials .................................................................................................................... 11
2.2. Experiment Procedure ...................................................................................................... 11
2.3. Observation Data ............................................................................................................... 12

CHAPTER III DATA PROCESSING .............................................................................................. 14

3.1. The Effect of Reflux Ratio to The Purity of the Product ............................................... 14
3.2. Theoretical Number of Stages .......................................................................................... 17
3.2.1. 100% Reflux .............................................................................................................. 20
3.2.2. 50% Reflux ................................................................................................................ 21
3.2.3. 33% Reflux ................................................................................................................ 21
3.2.4. 25% Reflux ................................................................................................................ 22
3.3. Tray Efficiency .................................................................................................................. 23
3.4. Relationship Between Product Quantity to the Reflux Ratio and Operating Time .... 23
3.5. Relationship Between Steam Flow Rate to the Reflux Ratio and Operating Time ..... 24

CHAPTER IV DATA ANALYSIS .................................................................................................... 26

4.1. Equipment and Materials Analysis .................................................................................. 26
4.2. Experiment Procedure Analysis ....................................................................................... 27
4.3. Calculation and Graph Analysis ...................................................................................... 27
4.1. Error Analysis .................................................................................................................... 30

CHAPTER V CONCLUSION ........................................................................................................... 31

REFERENCES .................................................................................................................................... 32

APPENDIX .......................................................................................................................................... 33

i
 LIST OF TABLES

Table 2.1 Observation Data..................................................................................................... 13

Table 3.1 Relationship of Mole Fraction for Every Component with Mixture Density ......... 14
Table 3.2 Calculation of Acetone Mole Fraction at 100% Reflux .......................................... 15
Table 3.3 Calculation of Acetone Mole Fraction at 50% Reflux ........................................... 16
Table 3.4 Calculation of Acetone Mole Fraction at 33% Reflux ........................................... 16
Table 3.5 Calculation of Acetone Mole Fraction at 25% Reflux ........................................... 16
Table 3.6 Antoine Constant of Acetone and Water ................................................................ 18
Table 3.7 Calculation Result for the Equlibrium Curve of Acetone-Water ............................ 18
Table 3.8 Calculation Result of the Theoretical Number of Stages ........................................ 23
Table 3.9 Tray Efficiency........................................................................................................ 23
Table 3.10 Relationship between Density to the Operating Time .......................................... 23
Table 3.11 Relationship between Steam Flow Rate to the Operating Time ........................... 25

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 LIST OF FIGURES

Figure 1.1 Fractional Distillation .............................................................................................. 7

Figure 1.2 Reflux Multistage Batch Distillation Tool .............................................................. 9
Figure 1.3 McCabe-Thiele Plotting Graph ............................................................................. 10
Figure 3.1 Relationship between Mixture Density and Mole Fraction Acetone .................... 15
Figure 3.2 Relationship between Time and Mole Fraction of Distillate for every Reflux Ratio
.......................................................................................................................................... 17
Figure 3.3 Relationship between Time and Mole Fraction of Bottom for every Reflux Ratio
.......................................................................................................................................... 17
Figure 3.4 Equilibrium Curve of Acetone-Water ................................................................... 19
Figure 3.5 Determination of the Number of Stages for 100% Reflux .................................... 20
Figure 3.6 Determination of the Number of Stages for 50% Reflux ..................................... 21
Figure 3.7 Determination of the Number of Stages for 33% Reflux ..................................... 22
Figure 3.8 Determination of the Number of Stages for 25% Reflux ..................................... 22
Figure 3.9 Relationship between Density to the Operating Time ........................................... 24
Figure 3.10 Relationship between Steam Flow Rate to the Operating Time .......................... 25

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 CHAPTER I

INTRODUCTION

1.1. Experiment Objectives

Below are the experiment objectives of the distillation practical.
• To learn about the effect of reflux ratio to the purity of the product
• To obtain the number of stages needed to separate acetone from the mixture of
acetone-water at certain operation condition (reflux ration and operating time)
• To determine the tray efficiency from the distillation equipment used
• To acknowledge the relationship between the product quantity and steam flow
rate with reflux ratio and operating time

1.2. Basic Theory

Distillation has been known as an important separation process in chemistry, industry,
and food science. Distillation is defined as a process involving the conversion of liquid into
vapor that is subsequently condensed back to liquid form. It is used to separate liquids from
non-volatile solids, as in separation of alcoholic liquors from fermented materials, or in the
separation of two or more liquids having different boiling points with high steam pressure, as
in the separation of gasoline, kerosene, and lubrication oil from crude oil. Moreover, other
industrial applications include the processing of such chemical products as formaldehyde and
phenol and the desalination of seawater. This processes have been utilized by the earliest
experimentalist; such as Aristotle (384-322 BC) which mentioned that pure water is able to be
made by the evaporation of seawater (Gregersen, n.d.).
Distillation column known for their ability for separation and purification. However,
this process occurs by the help from the equipped system. This basic operation requires the use
of a still or retort boilers in which liquid is heated, a condenser to cool the vapor, and a receiver
to collect the distillate. In heating a mixture of substances, the most volatile or the lowest
boiling point distils first, and the others subsequently or even not at all. For laboratory use, the
apparatus is commonly made of glass and connected with corks, rubber bungs, or ground-glass
joints. For industrial applications, larger equipment of metal or ceramic is employed.

4
 There are some factors affecting distillation operation, namely:
1. Feed Conditions
The state of the feed mixture and feed composition affects the operating lines
and hence the number of stages required for separation. It also affects the location of
feed tray. During operation, if the deviations from design specifications are excessive,
then the column may no longer be able to handle the separation task. Thus, to overcome
the problems associated with the feed, some column is designed to have multiple feed
points when the feed is expected to containing varying amounts of components.

2. Reflux Conditions
As the reflux ratio increased, the gradient of operating line for the rectification
section moves toward a maximum value of 1. Physically, this means that more and
more liquid that is rich in the volatile components are recycled back into the column.
Separation then becomes better and thus less trays are needed to achieve the same
degree of separation. On the other hand, when reflux ratio decreased, the operating line
moves towards the equilibrium line. This means more trays are required.

3. Vapor Flow Conditions

a. Foaming
Adverse vapor flow conditions can cause foaming. Foaming refers to the
expansion of liquid due to passage of vapor or gas. Although it provides high
interfacial liquid-vapor contact, excessive foaming often leads to liquid build up on
trays. In some cases, foaming may overload and thus mixes with liquid on the tray
above. Foaming may occur either due to the physical properties of the liquid
mixtures or due to the tray designs and condition which lead to the reduction of
efficiency.

b. Entrainment
Entrainment refers to the liquid carried by vapor up to the try above and caused
by high vapor flow rate. It is detrimental because the tray efficiency is reduced due
to lower volatile material is carried to the higher volatile materials tray. Which
means this will contaminate the high purity distillate. Moreover, excessive
entrainment can lead to flooding.

5
 c. Weeping or Dumping
The phenomenon of weeping or dumping is occurring due to low vapor flow.
The pressure exerted by the vapor is insufficient to hold up the liquid on the tray.
Therefore, liquid starts to leak through perforations, which then lead to dumping.
Dumping is a phenomenon where liquid on all trays will crash through to the base
of the column, through a domino effect, and the column will have to be re-started
and the separation process to start back from the beginning. Weeping is indicated
by a sharp pressure drop in the column.

d. Flooding
Flooding is the result from excessive entrainment, which caused by excessive
vapor flow, causing the liquid to be entrained in the vapor up the column. The
increased in pressure from excessive vapor also backs up the liquid in the down
comer, causing an increase in liquid hold up on the plate above. Depending on the
degree of flooding, the maximum capacity of the column may be severely reduced.
If weeping is indicated by a sharp pressure drop, flooding is recognized by sharp
increases in column differential pressure.

4. Column Diameter
Vapor flow condition is dependent on column diameter. Weeping determines
the minimum vapor flow required while flooding determines the maximum vapor flow
allowed, hence the column capacity. Thus, if the column diameter is not sized properly,
the column may not perform well, and problems will occur. The desired duties may not
be achieved.

5. State of Trays and Packings

The number of trays required for a particular separation duty is determined by
the efficiency of the plate, and the packings if packings are used. Thus, any factors that
cause a decrease in tray efficiency will also change the performance of the column.
Tray efficiencies mainly affected by fouling, tear, and corrosion, and the rates of which
these occur depends on the properties of the liquids being processed.

6
 There are a few types of distillation used in industrial which mainly depends on the
components of mixtures being separated, these includes:
a. Simple Distillation
Simple distillation involves heating the liquid mixture to the boiling point and
immediately condensing the resulting vapor. This method is effective for mixtures
where in boiling points of the liquids are considerably different, in which a minimum
difference of 250C. The purity of the distillate than is governed by Raoult’s Law.
b. Fractional Distillation
Fractional distillation is often used to separate mixtures of liquids that have
similar boiling points. It involves several vaporization-condensation steps, that takes
place in a fractioning column. This process of distillation is widely known as
rectification. Rectification process needs a round bottom flask or distilling flask, a
source of heat, receiving flask to collect the condensed vapor, fractioning column,
thermometer to measure temperature in the distilling flask, condenser, and standard
glassware. When heated, the liquid mixture is converted into vapor that rise into the
fractioning column. the vapor then cool down and condense on the condenser. The hot
vapor emanating from the distilling flask now heat the condensed vapor, creating new
vapor and moving it along the column and eventually yielding a higher purity sample
of the more volatile component of the mixture (Helmenstine, 2020).

Figure 1.1 Fractional Distillation

(BYJU'S, 2019)

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 c. Steam Distillation
Steam distillation is often used to separate heat-sensitive components in a
mixture. This process is done by passing steam through the mixture, which slightly
heated, to vaporize some of it. The process establishes a high heat-transfer rate without
the need for high temperatures. The resulting vapor is condensed to afford the required
distillate. Steam distillation mainly used to obtain essential oils and herbal distillates
from several aromatic flowers or herbs.
d. Vacuum Distillation
Vacuum distillation is the type of distillation which ideal for separating
mixtures of liquids with very high boiling points. In order to boil these compounds,
heating to high temperature is an inefficient method. Therefore, the pressure of the
surroundings is lowered instead. This was done to enables the component to boil at
lower temperatures. Once the vapor pressure of the component is equal to the
surrounding pressure, it is converted to vapor. These vapors are then condensed and
collected as the distillate. The vacuum distillation method is also used to obtain high
purity samples of compounds that decompose at high temperatures.
e. Air-Sensitive Vacuum Distillation
This kind of distillation is used for compounds that are sensitive to air and
readily react with it. The vacuum distillation process is carried out, but the vacuum
must be replaced with an inert gas once the process is complete.
f. Short Path Distillation
Short path distillation is used to purify a small quantity of a compound that is
unstable at high temperatures. This distillation process is done under lowered pressure
levels and generally involves the distillate to travel a very small distance before being
collected. This is why it is being called as the “short path”. The reduced distance
travelled by the distillate in this method also reduces the wastage along the walls of the
apparatus.
g. Zone Distillation
The process of zone distillation involves the partial melting of a substance and
the condensation of the resulting vapor to obtain a pure distillate. This is carried out in
a long container with the help of a zone heater.

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McCabe-Thiele Method
In practice, there are two methods of distillation. The first method is based on steam
production, the steam was produced by heating the liquid mixture apart and then condensing
the steam and not allowing the condensate liquid to return to the column. This method of
distillation is called as the distillation without reflux. The second method on the other way, can
be done by returning some of the condensed steam so that it can make contact with the vapor
that goes into the condenser or in other words, reflux is carried out on this distillation so that
the product obtained can have higher purity. Both of these methods can be carried out in a
continuous or batch process.
The practicum of distillation will be done by using a batch process, where there is no
flow in and out of the system during the process. Distillation with a simple batch process
usually will not produce a good separation unless there is a big difference in each of the
components boiling point. In many cases, the rectification column completed with a reflux are
used to improve the performance of the distillation. The illustration for this process can be seen
in Figure with the statement W denoted the amount of feed in the boiler with liquid mole
fraction of xW, while V as the amount of vapor with steam mole fraction of yD. Furthermore,
the steam then condensed and divided into two, L as the amount of the reflux and D denoted
the number of products with the same liquid mole fraction xD.

Figure 1.2 Reflux Multistage Batch Distillation Tool

(Modul Praktikum Unit Operasi Proses II, 2013)

Distillation operation in a batch system with reflux can be analyze with McCabe-Thiele
diagram, with a formula of
𝑅' 𝑥'
𝑦"#$ = 𝑥" +
𝑅' + 1 𝑅' + 1

9
Where 𝑦"#$ as the mole fraction of volatile components in the vapor point in the tray n+1, 𝑥"
as the mole fraction of volatile components of liquid in tray, 𝑥' as mole fraction of volatile
components in distillate, and 𝑅' as the reflux ratio which being used as the comparison
between the amount of liquid went back to the column and the liquid that taken as the product
(L/D).
The operation line obtained from the McCabe-Thiele equation; it can be used to find
the number of trays that are needed in theory by plotting the equilibrium curve. Moreover, the
tray efficiency can be calculated by:
𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑇𝑟𝑎𝑦
𝜂= ×100%
𝐴𝑐𝑡𝑢𝑎𝑙 𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑇𝑟𝑎𝑦

Figure 1.3 McCabe-Thiele Plotting Graph

(Modul Praktikum Unit Operasi Proses II, 2013)

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 CHAPTER II

EXPERIMENT AND OBSERVATION DATA

2.1. Equipment and Materials

2.1.1. Equipment
The equipment needed for the distillation practical are:
• Batch distillation with reflux
• Pycnometer
• Volume gauge tube
• Scale
• Heat resistant gloves
• Stopwatch

2.1.2. Materials
The materials needed for the distillation practical are:
• Mixture of acetone and water
• Cooling water

2.2. Experiment Procedure

There are several procedure needs to be done in the distillation practical, which are:
1. Preparing 5L solution of acetone and water with 10% mol of acetone
2. Pouring the solution into the feed tank.
3. Activating the cooling water to 2500 mL/min.
4. Activating the heater and set the temperature to 80°C using the temperature
control.
5. Using the potentiometer to set the reflux to 100%
6. Opening V3 to make the product flow back from product tank to feed tank
7. Recording the temperature of feed tank when steam and liquid started to flow
into the column, turn off the heater.
8. Taking 10 mL of sample from feed tank using beaker glass and pycnometer
then cool it down.
9. After the sample is cold enough, testing the mass and density of the sample
and record it.

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 10. Turning on the heater again and set the reflux to 50% using potentiometer
column and feed tank and set it to 1:1, close of V3
11. Turning on the stopwatch, when steam and liquid started to flow into the
column
12. Using the decanter to stabilize the amount of distillate formed
13. Taking 10 ml sample from feed tank and product tank for 0, 5, 10, and 15
minutes. Using pycnometer directly for the product distillate and using beaker
to help when measuring the bottom feed.
14. Recording and calculating the density of samples when the sample is cold.
15. Turning off the heater and open V3, let it be until all the liquid flow back into
feed tank.
16. Performing step 10 – 16 for reflux variation of 33% and 25% by setting the
potentiometer for column and product tank to 1:2 and 1:3
17. After the experiment is finished, turning back the temperature setting to 30 °C,
wait about 5 minutes before the equipment can be turned off
18. Cooling water can be closed after the equipment is turned off
19. When the feed tank has cooled down, opening the bottom valve to empty the
tank.
20. Cleaning the pycnometer and beaker glass before storing it

2.3. Observation Data

Below are the literature data obtained for the distillation practical.
• Mass of empty pycnometer distillate = 15.85 grams
• Volume of pycnometer distillate = 10 ml
• Mass of empty pycnometer bottom = 16.42 grams
• Volume of pycnometer bottom = 10 ml
• Density of aquadest = 0.96 gram/cm3
• Density of acetone = 0.721 gram/cm3

Shown below are the observation data of the distillation practical for four reflux
percentages.

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 Table 2.1 Observation Data

Mass of Distillate Mass of Bottom +

Time Temperature
Reflux + Pycnometer Pycnometer
(minutes) (oC)
(gram) (gram)
0 55 25.1 26.18
5 64 24.1 26.23
100%
10 65 24.08 26.28
15 67 24.01 26.34
0 61 24.7 26.2
5 63 24.45 26.24
50%
10 65 24.35 26.32
15 70 24.29 26.36
0 65 24.53 25.54
5 70 24.47 26.25
33%
10 72 24.31 26.38
15 74 24.25 26.38
0 65 24.36 26.29
5 70 24.28 26.32
25%
10 74 24.22 26.37
15 75 24.15 26.4

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 CHAPTER III

DATA PROCESSING

3.1. The Effect of Reflux Ratio to The Purity of the Product

Below are several steps to find the effect of reflux ratio to the purity of the product.
a) Calculating the Density of Water-Acetone Mixture
The mixture density is needed to calculate the acetone mole fraction. Below
is the formula used to calculate the mixture density.
• Distillate density
𝑚A
𝜌A =
𝑉A
Ø 𝑚A = mass of filled pycnometer – mass of empty pycnometer (g)
Ø 𝑉A = distillate volume = 10 mL

• Bottom density
𝑚C
𝜌C =
𝑉C
Ø 𝑚C = mass of filled pycnometer – mass of empty pycnometer (g)
Ø 𝑉C = distillate volume = 10 mL

b) Calculating the Acetone Mole Fraction

The acetone mole fraction is calculated using the data of mixture density of
water-acetone by using the molecular mass of acetone and water.
Ø Molecular mass of acetone = 58.08
Ø Molecular mass of water = 18.015

The table shown below are the calculation of mixture density of water-
acetone for every mole fraction.

Table 3.1 Relationship of Mole Fraction for Every Component with Mixture Density

Mole Fraction Acetone Mole Fraction Water Mixture Density

0 1 0.9982071
0.1 0.9 0.924990378
0.2 0.8 0.874314213

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 0.3 0.7 0.837158103
0.4 0.6 0.808748267
0.5 0.5 0.786321689
0.6 0.4 0.768168288
0.7 0.3 0.753172976
0.8 0.2 0.740577598
0.9 0.1 0.729848693
1 0 0.7206

From the table above, we can plot the graph of mixture density and mole fraction
acetone.

Figure 3.1 Relationship between Mixture Density and Mole Fraction Acetone

From the graph, the equation obtained is 𝑦 = 14.252𝑥 H − 27.809𝑥 + 13.587. From
this equation, we can find the mole fraction of acetone in the distillate and bottom, where the
calculation is presented in the table below.

• 100% Reflux

Table 3.2 Calculation of Acetone Mole Fraction at 100% Reflux

t (min) T (oC) 𝒎𝑫 (g) 𝝆𝑫 (g/ml) 𝒙𝑫 𝒎𝑩 (g) 𝝆𝑩 (g/ml) 𝒙𝑩

0 55 9.25 0.925 0.0580425 9.76 0.976 0.0215292

5 64 8.25 0.825 0.3448425 9.81 0.981 0.02194
10 65 8.23 0.823 0.3534859 9.86 0.986 0.0230634
15 67 8.16 0.816 0.3846357 9.92 0.992 0.0253521

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 • 50% Reflux
Table 3.3 Calculation of Acetone Mole Fraction at 50% Reflux

t (min) T (oC) 𝒎𝑫 (g) 𝝆𝑫 (g/ml) 𝒙𝑫 𝒎𝑩 (g) 𝝆𝑩 (g/ml) 𝒙𝑩

0 55 8.85 0.885 0.1385577 9.78 0.978 0.0216080
5 64 8.6 0.86 0.2120392 9.82 0.982 0.0221076
10 65 8.5 0.85 0.24642 9.9 0.99 0.0244752
15 67 8.44 0.844 0.2684167 9.94 0.994 0.0263431

• 33% Reflux
Table 3.4 Calculation of Acetone Mole Fraction at 33% Reflux

t (min) T (oC) 𝒎𝑫 (g) 𝝆𝑫 (g/ml) 𝒙𝑫 𝒎𝑩 (g) 𝝆𝑩 (g/ml) 𝒙𝑩

0 55 8.68 0.868 0.1865868 9.12 0.912 0.0792075

5 64 8.62 0.862 0.2055051 9.83 0.983 0.0223038
10 65 8.46 0.846 0.2609704 9.96 0.996 0.0274480
15 67 8.4 0.84 0.2836512 9.96 0.996 0.0274480

• 25% Reflux
Table 3.5 Calculation of Acetone Mole Fraction at 25% Reflux

t (min) T (oC) 𝒎𝑫 (g) 𝝆𝑫 (g/ml) 𝒙𝑫 𝒎𝑩 (g) 𝝆𝑩 (g/ml) 𝒙𝑩

0 55 8.51 0.851 0.2428537 9.87 0.987 0.0233736

5 64 8.43 0.843 0.2721825 9.9 0.99 0.0244752
10 65 8.37 0.837 0.2953764 9.95 0.995 0.0268813
15 67 8.3 0.83 0.3237328 9.98 0.998 0.0286670

Where:
Ø t : time (min)
Ø T : temperature (oC)
Ø 𝑚' : mass of distillate
Ø 𝜌' : density of distillate
Ø 𝑥' : acetone mole fraction in distillate
Ø 𝑚S : mass of bottom
Ø 𝜌S : density of bottom
Ø 𝑥S : acetone mole fraction in bottom

16
 From the calculation, we can plot the graph of time and mole fraction of distillate and
also time and mole fraction of bottom.

Figure 3.2 Relationship between Time and Mole Fraction of Distillate for every Reflux Ratio

Figure 3.3 Relationship between Time and Mole Fraction of Bottom for every Reflux Ratio

3.2. Theoretical Number of Stages

To determine the theoretical number of stages, we need to make the equilibrium curve
of acetone-water. From the literature, the Antoine constant for acetone and water is presented
in the table below.

17
 Table 3.6 Antoine Constant of Acetone and Water
Component A B C Boiling Point (oC)
Acetone 7.2316 1277.03 237.23 56
Water 8.07131 1730.63 233.426 100

To calculate the 𝑃UVW , we can use the following formula:

𝐵
𝑙𝑜𝑔𝑃UVW = 𝐴 −
𝐶+𝑇

S
𝑃UVW = 10[\]#^
where:
• 𝑃UVW : vapour pressure of the components (mmHg)
• 𝑇 : temperature (oC)
• 𝐴, 𝐵, 𝐶 : Antoine equation for every components

The next step is to find the value of x and y* by using the following formula:
𝑃^ − 𝑃V`a
𝑥=
𝑃VUbWc" − 𝑃V`a

𝑃VUbWc" 𝑥
𝑦∗ =
𝑃^

where:
• 𝑃VebWc"b : vapour pressure of acetone (mmHg)
• 𝑃fVWba : vapour pressure of water
• 𝑃^ : total pressure of mixture
• 𝑥 : liquid mole fraction of acetone
• 𝑦∗ : vapour mole fraction of acetone

Below is the calculation to construct the equilibrium curve of acetone-water, which is

presented in the table.
Table 3.7 Calculation Result for the Equlibrium Curve of Acetone-Water

T (oC) P aseton (mmHg) P water (mmHg) x y*

56 752.5831191 123.5335748 1 1
58 805.4845282 135.7754738 0.932083152 0.987866523
60 861.3167587 149.0384192 0.857756788 0.972105653

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 62 920.1942548 163.3906107 0.78832785 0.954493103
64 982.2336595 178.9035524 0.723359479 0.934878984
66 1047.55378 195.6521392 0.662456596 0.91310383
68 1116.275548 213.7147418 0.605261445 0.888998094
70 1188.521984 233.1732906 0.551449657 0.862381632
72 1264.418152 254.1133586 0.500726755 0.833063157
74 1344.09112 276.6242422 0.452825064 0.800839669
76 1427.669912 300.7990412 0.407500957 0.765495863
78 1515.285467 326.7347363 0.364532411 0.726803507
80 1607.070587 354.5322655 0.32371683 0.684520784
82 1703.15989 384.2965982 0.284869102 0.638391617
84 1803.689763 416.1368073 0.24781987 0.58814495
86 1908.798306 450.1661395 0.212413978 0.533494001
88 2018.625282 486.5020829 0.178509089 0.474135475
90 2133.312067 525.2664328 0.145974444 0.40974874
92 2253.001589 566.5853549 0.114689743 0.339994966
94 2377.83828 610.5894458 0.084544152 0.264516212
96 2507.968017 657.4137916 0.055435397 0.182934478
98 2643.538064 707.1980231 0.027268959 0.094850698
100 2784.697018 760.0863692 0 0

Figure 3.4 Equilibrium Curve of Acetone-Water

Determining the number of stage for each reflux can be done by using the operating
line which intersects with the distillate fraction and the equilibrium curve of acetone-water.

19
The operating line equation can be expressed by the total mass balance and the component
mass balance, which are presented below.
𝑉"#$ = 𝐿" + 𝐷
𝑉"#$ 𝑦"#$ = 𝐿" 𝑥" + 𝐷𝑥'

From both equation presented earlier, we can obtained the following equation:
𝐿 𝐿
𝑦"#$ = 𝑥" + 1 − 𝑥
𝑉 𝑉 '

With the following equation:

𝐿
𝐿 𝐷 𝑅
= =
𝑉 1+ 𝐿 1+𝑅
𝐷

Hence, the equation can be written as:

𝑅 𝑥'
𝑦"#$ = 𝑥" +
𝑅+1 𝑅+1

3.2.1. 100% Reflux

1 0.285252
𝑦"#$ = 𝑥" +
1+1 1+1

0.285252
𝑦"#$ = 0.5 𝑥" +
2

𝑦"#$ = 0.5 𝑥" + 0.142626

Figure 3.5 Determination of the Number of Stages for 100% Reflux

20
3.2.2. 50% Reflux

0.5 0.216358
𝑦"#$ = 𝑥" +
0.5 + 1 0.5 + 1

0.216358
𝑦"#$ = 0.3333 𝑥" +
1.5

𝑦"#$ = 0.3333 𝑥" + 0.14423867

Figure 3.6 Determination of the Number of Stages for 50% Reflux

3.2.3. 33% Reflux

0.33 0.234178
𝑦"#$ = 𝑥" +
0.33 + 1 0.33 + 1

0.234178
𝑦"#$ = 0.2481 𝑥" +
1.33

𝑦"#$ = 0.2481 𝑥" + 0.17607368

21
 Figure 3.7 Determination of the Number of Stages for 33% Reflux

3.2.4. 25% Reflux

0.25 0.283536
𝑦"#$ = 𝑥" +
0.25 + 1 0.25 + 1

0.283536
𝑦"#$ = 0.2 𝑥" +
1.25

𝑦"#$ = 0.2 𝑥" + 0.226829

Figure 3.8 Determination of the Number of Stages for 25% Reflux

22
 From all the graph presented earlier, we can have obtained the theoretical number of
stages for every reflux.

Table 3.8 Calculation Result of the Theoretical Number of Stages

Reflux Theoretical Number of Stages

100% 2
50% 1
33% 1
25% 1

3.3. Tray Efficiency

The tray efficiency can be calculated using the following formula.

𝜂W total of theoretical tray
𝜂= = ×100%
𝜂V total of actual tray

Table 3.9 Tray Efficiency

Total of Total of
Reflux Tray Efficiency (%)
Theoretical Tray Actual Tray
100% 2 9 22.22222222
50% 1 9 11.11111111
33% 1 9 11.11111111
25% 1 9 11.11111111

3.4. Relationship Between Product Quantity to the Reflux Ratio and Operating Time

The product quantity is calculated from the density, which is obtained from the mass
of distillate divided by the volume of distillate.

Table 3.10 Relationship between Density to the Operating Time

𝝆𝑫 (g/ml)
Time (min) Total Reflux Reflux Reflux
Reflux 50% 33% 25%
0 0.925 0.885 0.868 0.851
5 0.825 0.86 0.862 0.843
10 0.823 0.85 0.846 0.837
15 0.816 0.844 0.84 0.83

23
 Figure 3.9 Relationship between Density to the Operating Time

3.5. Relationship Between Steam Flow Rate to the Reflux Ratio and Operating Time
The steam flow rate can be calculated with the following formula.

𝑅+1
𝑉= 𝑥v − 𝑥C`
𝑡
where:
• 𝑉 : steam flow rate
• 𝑅 : reflux ratio (%)
• 𝑡 : time (minutes)
• 𝑥v : initial mole fraction
• 𝑥C` : mole fraction in bottom

24
 Table 3.11 Relationship between Steam Flow Rate to the Operating Time

Reflux Ratio t 𝒙𝟎 𝒙𝒃𝒊 V (mol/min)

5 0.0215292 0.186022742
10 0.0219400 0.092929207
100% 0.48658601
15 0.0230634 0.061803015
20 0.0253521 0.046123388
5 0.0216080 0.136029687
10 0.0221076 0.067939891
50% 0.47504026
15 0.0244752 0.045056506
20 0.0263431 0.033652289
5 0.0792075 0.108643168
10 0.0223038 0.061889771
33% 0.48764045
15 0.0274480 0.040803728
20 0.0274480 0.030602796
5 0.0233736 0.109907419
10 0.0244752 0.054816008
25% 0.46300326
15 0.0268813 0.036343497
20 0.0286670 0.027146016

Figure 3.10 Relationship between Steam Flow Rate to the Operating Time

25
 CHAPTER IV

DATA ANALYSIS

4.1. Equipment and Materials Analysis

The main equipment of batch distillation column are tank, reboiler, condenser,
potentiometer, the columns, and cooling system. For the tank, there are 2 types of tank which
are feed tank for product tank. The needs of both tanks are different therefore the material used
for each tank also differ. For the feed tank the important thing is it can hold of feed (in this case
acetone and water mixture) for a long time without being damaged. The feed tank must also be
able to withstand heat of the feed inside of it. With those things in mind, the selected material
for the feed tank is steel. For the product tank, in this experiment the important thing is seeing
the liquid flow into the product tank, so viewability is prioritized. The material of the product
tank does not need to be as strong as feed tank as the temperature and the amount of solution
inside of it significantly different with the product tank contain solution with less temperature
and volume than feed tank. After considering those aspects, the product tank material is glass
or some more transparent plastics to reduce cost and to improve viewability, thus decreasing
the chance of human error. The principle that applies to selecting material of product tank also
apply to column as the column also needs to be transparent so that the process can be viewed
easily. In this experiment, the reboiler and condenser used are connected to the column as the
first and last column respectively. The size is also quite small as the volumetric flow rate of
feed in this experiment are not high. For cooling system, water is used as water is cheap, save,
and with proper equipment the flowrate is easily controllable. The desired cooling temperature
in this experiment is also not that low (at the lowest about 30°C) making normal water quite
ideal for this experiment in both safety and cooling ability.
For the supportive equipment of this experiment, there are beaker glass, pycnometer,
electrical balance, stopwatch and glove. Glove and beaker glass are more of a safety equipment.
Gloves are used to protect the hand from direct contact towards the solution and heat. Beaker
glass offer protection to the student when attempting to get the bottom feed solution which
have a high temperature. Stopwatch is used to measure time for each viewing checkpoint.
Pycnometer is a small bottle with a very precise measurement of the volume that it can contain,
it is used to help getting an accurate density measurement of the samples. Do not forget, to get
a correct measurement with pycnometer the pycnometer needs to be measured for its mass
before putting solution inside of it. Electrical balance is used to get an accurate measurement

26
of the sample’s mass. With the help of both electrical balance and pycnometer, an accurate
density of each sample can be measured.
For the material used in this experiment there is only acetone and water mixture, both
are polar. This polar mixture can be separated easily therefore it is suitable for this experiment.
In this mixture, the heavier component is water.

4.2. Experiment Procedure Analysis

The laboratory of batch distillation is done with the objective of finding out the
relationship between reflux ratio and operation time with flow rate, distillate and bottom’s mole
fraction, and the number of trays. To achieve the objectives, the first procedure to do is to put
the feed which is 5 litres mixture of acetone and water into the feed tank. After that, to make
the distillation process going, there is a need to activate heater and get the heat into the system.
In this experiment, the controlled variables are time (minutes) and the reflux of the system.
Data gathering is obtained at minute 0, 5, 10, and 15 to view the process of distillation more
clearly. Reflux variation is done to observe the effect of reflux (enriching) towards final product
density and at the end, the theoretical stage and efficiency of the system. The data are taken
directly using pycnometer for the product and using the help of beaker glass for the feed, this
is because the volume and temperature of the feed is higher making it unsafe for the practitioner
to directly using pycnometer as the mixture might pour into their hands. Still, after beaker is
used, some of the mixture inside of it will be safely transferred into the pycnometer. The data
that are obtained throughout the procedure are column temperature when the sample are taken,
volume of the distillate, and mass of the bottom. The density, stages, and other graph will be
calculated from the said data.

4.3. Calculation and Graph Analysis

4.3.1. The Effect of Time to Mole Fraction of Distillate and Bottom

As time goes by, the graph of time vs mole fraction of distillate shows that the mole
fraction of distillate increased. Which suits the theory in which the mixture that comes from
the distillation column will have higher content of acetone due to the repeated process of
distillation. As we know, the distillation process is meant to separate water from the acetone to
get higher purity level of acetone. For each of the reflux ratio, the longer the time, the higher
the fraction mole of distillate achieved. Moreover, from the graph, it is shown that for reflux

27
ratio equal to 100%, they have the highest mole fraction of distillate, this is due to for an
existing column where the number of trays used is fixed, to get higher distillate mole fraction,
we must increase the reflux ratio. Because the higher the reflux ratio means the more of the
distillate product goes back to the distillation column, and hence produced higher purity level.
However, in our experimental result graph, the reflux ratio at 25% has higher mole fraction
than the reflux ratio at 33% and 50%. In addition, for reflux ratio of 50% yield the lowest mole
fraction of distillate.
For graph between time vs mole fraction of bottom, they also shared a similar result in
which as the times get longer, the greater the mole fraction in bottom. Although in this case,
there is only a slightly different in each of the reflux ratio, except for reflux ratio of 33% that
drop significantly in the first five minutes, that might be due to the errors occur in the
experiment. However, in the theory, the mole fraction of acetone in the bottom should get lower
and lower as time passed by because acetone should go to the distillate. From another point,
the graph suits the theoretical concept in which, the lower the reflux ratio will result to the
higher mole fraction of bottom. This is due to for higher reflux ratio, more acetone will make
it to the distillate.

4.3.2. Theoretical Number of Stage

In this experiment, we used McCabe-Thiele method to determine the number of
theoretical trays in the distillation column. This method uses the equilibrium curve diagram to
determine the number of theoretical trays required to achieve a desired degree of separation.
To get this curve, some information regarding to the feed condition, both temperature and
compositions, distillate and bottom compositions, and the reflux ratio. After all the parameter
obtained, we will then be able to create the equilibrium curve, and by calculating the rectifying,
feed and stripping line, with the help from Antoine constant, we will then be able to determine
each of the number of theoretical trays for each of the reflux ratio. From the calculation, it can
be concluded that in our experiment, the lower the reflux ratio will need smaller number of
trays. All of the reflux ratios, from 25%, 33%, and 50% need 1 tray, except for reflux ratio
100% needs 2 trays. However, based on the theory the greater the reflux ratio should result in
the lesser the number of theoretical trays.

4.3.3. Tray Efficiency

The value of tray efficiency is got from dividing the number of theoretical trays by the
actual number of trays and multiplying by 100%. This means that we want to know how

28
efficient our distillation process by comparing the actual number of trays we used to the one
we supposedly have (the theoretical one). The number of trays used is equal to 9 trays, thus,
the tray efficiencies for our reflux ratio are 22.222% for 100% reflux ratio and 11.111% for
reflux ratio of 25%, 33%, and 50%. Form here, we considered that our experiment tray
efficiency is low and one of the causes is due to an imperfect process occurred in the mass and
heat transfer inside the distillation column. Theoretically, the steam inside the distillation
column should be distributed evenly to ensure a maximum contact between steam and the
mixtures to reach the desired amount and time of separation. However, in this experiment, the
amount of heat distributed in different level of trays might have affected the vaporizing
processes, and thus, resulted to the inefficiency of the trays.

4.3.4. The Effect of Density to the Operating Time
From the graph between product quantity to the reflux ratio versus the operating time,
we can observe that the longer the time will result to the decrease of the density of the product.
The density is obtained by dividing the number of products produced by 10 mL of product.
This means, our experiment has suited the theoretical, in which, the longer the time means that
the rate of separation has already decreased. Because, at the initial condition, the separation
processes between acetone and water occurred so great due to the low boiling point of acetone.
As time passed, the number of acetones left in the distillation column has decreased because
mostly has ended at the distillate.

4.3.5. Relationship Between Steam Flow Rate to The Reflux Ratio and Operating Time
From the graph between the steam flow rate versus the operating time, it is shown that
the longer the time will make the steam flow rate to decrease. This graph is correct according
to the theory, in which, the longer the time will result to the decrease amount of acetone inside
the distillation column, therefore, the steam flow rate will decrease because the amount of
compound evaporating has been reduced. Moreover, the reflux ratio shows a similar figure
from each other, however, reflux ratio of 100% still hold the highest flow rate followed
sequentially by reflux ratio of 50%, 33%, and 25%. This is due to the higher the reflux ratio
means the more amount of product goes back to the distillation tank to go through a reflux
distillation and ensure the purity.

29
4.1. Error Analysis
In the experiment, the human error that easily occur is the inaccuracy of determining 0
minutes. This can slightly skew the result all the way until 15 minutes. To reduce this error,
much concentration is needed at the start of experiment, and if able there are more than one
person who observe the change for 0 minutes. The other technical aspect than can affect human
error in the lab is time. As time for the experiment is limited, the practitioner sometimes started
new variation of the experiment without waiting for all the condition to turn stable. This might
affect the result as impurity will be present when the previous variation of this experiment is
not considered completed. This is because the starting point of the new variation will be
different than what it is thought to be and will cause some mistakes as the experiment
progresses. The next error that can happen is when using pycnometer, as the volume is very
small some sample might drip outside of pycnometer wall, and these droplets must be wiped
off to get an accurate reading of mass for the specified pycnometer volume.

30
 CHAPTER V

CONCLUSION

From this distillation practical, several conclusions can be drawn which are presented below.
• Distillation is a process consist of the separation of liquid mixtures based on their
boiling point.
• Distillation process are equipped with boilers to heat the mixtures, distillation column
as the place for separation, condenser to condense the steam and distillate to keep the
condensed steam.
• Liquid with lower boiling point will be brought by the steam to the condenser which
then end as a distillate, where liquid with high boiling point will ends at the bottom.
• The higher the reflux ratio means the higher the purity of the fluid can be achieved.
• The longer the time will result to the increase of the mole fraction of the distillate and
the decrease of the mole fraction in the bottom.
• The higher the reflux ratio will give better tray efficiency and a smaller number of trays
will be needed.
• The longer the time has passed, the slower the steam flow rate due to most of the
substance has ended in the distillate.
• The tray efficiencies achieved in this experiment for reflux ratio of 100%, 50%, 33%,
and 25% are 22.22%, 11.11%, 11.11%, and 11.11%

31
 REFERENCES

Gregersen, E. (n.d.). BRITANNICA. Retrieved from Distillation :

https://www.britannica.com/science/distillation
Helmenstine, A. M. (2020). ThoughtCo. Retrieved from What is Distillation? Chemistry
Definition : https://www.thoughtco.com/what-is-distillation-601964
BYJU'S. (2019). Retrieved from Distillation: https://byjus.com/chemistry/distillation/
Modul Praktikum Unit Operasi Proses II. (2013).

32
 APPENDIX

Below is the pre-test of the distillation practical, which consist of two questions.

Questions
1) Explain the experiment objectives and procedure of the distillation practical
2) How to dilute 75% w/v technical acetone to 10% v/v acetone-water as feed from a
distillation batch that have the capacity of 5 Liter

Answers
1) The experiment objectives of the distillation practical are:
• To learn about the effect of reflux ratio to the purity of the product
• To obtain the number of stages needed to separate acetone from the mixture of
acetone-water at certain operation condition (reflux ration and operating time)
• To determine the tray efficiency from the distillation equipment used
• To acknowledge the relationship between the product quantity and steam flow
rate with reflux ratio and operating time

The procedure of the distillation practical are:

1. Preparing 5L solution of acetone and water with 10% mol of acetone
2. Pouring the solution into the feed tank.
3. Activating the cooling water to 2500 mL/min.
4. Activating the heater and set the temperature to 80°C using the temperature
control.
5. Using the potentiometer to set the reflux to 100%
6. Opening V3 to make the product flow back from product tank to feed tank
7. Recording the temperature of feed tank when steam and liquid started to flow
into the column, turn off the heater.
8. Taking 10 mL of sample from feed tank using beaker glass and pycnometer
then cool it down.
9. After the sample is cold enough, testing the mass and density of the sample
and record it.

33
 10. Turning on the heater again and set the reflux to 50% using potentiometer
column and feed tank and set it to 1:1, close of V3
11. Turning on the stopwatch, when steam and liquid started to flow into the
column
12. Using the decanter to stabilize the amount of distillate formed
13. Taking 10 ml sample from feed tank and product tank for 0, 5, 10, and 15
minutes. Using pycnometer directly for the product distillate and using beaker
to help when measuring the bottom feed.
14. Recording and calculating the density of samples when the sample is cold.
15. Turning off the heater and open V3, let it be until all the liquid flow back into
feed tank.
16. Performing step 10 – 16 for reflux variation of 33% and 25% by setting the
potentiometer for column and product tank to 1:2 and 1:3
17. After the experiment is finished, turning back the temperature setting to 30 °C,
wait about 5 minutes before the equipment can be turned off
18. Cooling water can be closed after the equipment is turned off
19. When the feed tank has cooled down, opening the bottom valve to empty the
tank.
20. Cleaning the pycnometer and beaker glass before storing it

2) Below are the calculation to answer the second question.

10
× 5𝐿 = 0.5 𝐿
100
0.5 𝐿 × 𝑃VebWc"b = 𝑥 𝑘𝑔
𝑥 𝑘𝑔 = 75% 𝑤
𝑥
× 100 = 𝑡𝑜𝑡𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡
75
𝑇𝑜𝑡𝑎𝑙 − 𝑥 = 4𝑘𝑔
𝑥 𝑘𝑔 × 𝑃VebWc"b + 𝑦 𝑘𝑔 × 𝑃fVWba = 𝑡𝑜𝑡𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑎𝑐𝑒𝑡𝑜𝑛𝑒

𝑘𝑔
75% → 0.5 𝐿 × 0.721 𝐿 = 0.3605 𝑘𝑔
100%
100% → = 0.3605 ×
75%

34
 = 0.481 𝑘𝑔 (𝑡𝑜𝑡𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡)
= 0.481 𝑘𝑔 − 0.3605 𝑘𝑔
= 0.1205 𝑘𝑔


5 𝐿 = 𝑎𝑑𝑑𝑒𝑑 𝑤𝑎𝑡𝑒𝑟 + 𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒
𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 = 5 𝐿 − 𝑎𝑑𝑑𝑒𝑑 𝑤𝑎𝑡𝑒𝑟
0.3605 𝑘𝑔 0.1205 𝑘𝑔
𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 = +
𝑘𝑔 𝑘𝑔
0.721 𝐿 0.96 𝐿
𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 = 0.5 𝐿 + 0.1255 𝐿
𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 = 0.625 𝐿


𝑎𝑑𝑑𝑒𝑑 𝑤𝑎𝑡𝑒𝑟 = 5 𝐿 − 𝑡𝑒𝑐ℎ𝑛𝑖𝑐𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒
𝑎𝑑𝑑𝑒𝑑 𝑤𝑎𝑡𝑒𝑟 = 5 𝐿 − 0.625 𝐿
𝑎𝑑𝑑𝑒𝑑 𝑤𝑎𝑡𝑒𝑟 = 4.375 𝐿

35