Distillation

Chemical Engineering Department, Technological Institute of the Philippines-Manila, Manila, Philippines

[email protected], [email protected], [email protected],

[email protected],[email protected]

Abstract— In this laboratory investigation, batch distillation was employed for the investigation of purity
analysis and the separation of a binary mixture of ethanol and water. The utilization of batch distillation was
necessary due to the distinct boiling points of the two components. The process involved heating the mixture,
causing the constituents to evaporate, and then condensing the vapor to obtain distillate. The concentration of
distillate and the bottoms were graphically represented overtime on an x-y diagram depicting the ethanol
mixture.

Index Terms— batch distillation, ethanol-water, x-y diagram

,
1 INTRODUCTION 2.1.12 Volumetric Flask
2.1.13 Pipette
Distillation stands as a prevalent method for separating 2.1.14 Aspirator
liquid-vapor mixtures in industrial settings, accommodating 2.2 PROCEDURE
both continuous and batch systems. The fundamental 2.2.1. Check the unit or set-up (iron stand, column, iron
principle involves applying and withdrawing heat to clamp, hot plate, condenser, adaptor, florence flask, and
leverage variations in relative volatility among erlenmeyer flask)
components. Heat induces the vaporization of substances 2.2.2. Fill up the florence flask with a 50% ethanol-water
with lower boiling points and higher volatility, while less solution.
volatile components remain in liquid form. Challenges arise 2.2.3. Insert the inlet and outlet tubes for the water that
when dealing with mixtures of similar boiling points or will serve as the cooling medium.
azeotropic compositions due to their low relative 2.2.4. Turn on the hot plate, maintain the temperature by
volatilities. Consequently, specialized distillation adjusting between the boiling points of ethanol and
techniques become essential to effectively separate such water then start the timer.
challenging mixtures. 2.2.5. When the distillate starts to fall on the glass
receiver, measure the time and the volume by opening
2 MATERIALS AND METHODS the stopcock, This enables you to get the total reflux.
2.2.6. During frequent intervals, simultaneously take a
2.1 MATERIALS sample of the distillate and a sample from the glass
vessel; measure the temperature and specific gravity for
2.1.1 Distilling flask
each sample.
2.1.2 Erlenmeyer Flask
2.2.7. Continue up to eight data points,
2.1.3 Condenser
2.2.8. Record the data.
2.1.4 Adaptor
2.1.5 Beaker
2.1.6 Rubber tubing
2.1.7 Cork 3 EXPERIMENTAL SET-UP
2.1.8 Hot Plate
2.1.9 Thermometer
2.1.10 Iron stand and clamp
2.1.11 Refractometer
 Table 4.2 Refractometer Outcome for Trial 1
Time (minutes) % volume/volume

First Drop 1.7

10 1.9

20 2.0

30 2.2

40 2.5

50 2.7

60 2.9

70 3.2

80 3.5

Table 4.2 depicts the refractometry results for the initial

distillation setup show the ethanol-water ratio in the liquid
product over time, measured in five-minute intervals. The data
reveals that the ethanol content rises as the distillation process
continues. The boiling point of the first drop is 78 degrees
Celsius or 351.15 Kelvin.

Table 4.3 Refractometer Outcome for Trial 2

Time (minutes) % volume/volume

First Drop 1.8

10 2.0
4 RESULTS AND DISCUSSION
20 2.2
The following tables and figures show the results and calculation
from the distillation experiment which were obtained from using 30 2.4
a refractometer.
40 2.7
Table 4.1 Density and Temperature of Distillate
50 2.9
Set- ρ Feed
First EtOH EtOH Collected
up
Drop Solution Feed %v/v Waste 60 3.1
(°C) (mL) (mL)
70 3.5
1 78 0.8 500 0.5 3.5 465
7
80 3.7
2 79 0.8 500 0.5 3.7 463
75
3 81 0.8 500 0.5 3.8 462
79 Table 4.3 shows the refractometry results of the second
distillation set-up through the ethanol-water ratio of the liquid
Table 4.1 a simplified summary of the initial drop measurements product in percent weight in a constant interval of five minutes.
for ethanol boiling points in three different setups. It also includes As observed in the obtained data points, the ethanol content
density measurements for the distilled liquid in each setup. The increases as the duration of the distillation process goes by or in
table displays the feed compositions and the waste solution time. The boiling point of the first drop is 79 degrees Celsius or
collected during the distillation process. All three setups have 352.15 degrees Kelvin.
identical compositions and procedures.
Table 4.4 Refractometer Outcome for Trial 3
 Tempe Pa* Pa Pb* Pb Act. Act.
Time (minutes) % volume/volume
rature Coef. Coef
(K) ETO .
First Drop 1.9
H H2O
10 2.1 1 351.15 8881 6512 38564 2315 1.230 1.48
5.13 9.770 .2260 1.801 4 60
20 2.3 17 3 3 7
2 352.15 9245 6254 40205 3748 1.134 1.48
30 2.4 0.70 2.034 .0039 2.601 1 53
10 81 6
40 2.5 3 354.15 1000 6782 43663 3678 1.134 1.34
93.4 1.624 .3205 1.696 6 64
50 2.8 391 8 1 3

60 3.2 Table 4.6 Displays the determined saturated vapor pressures and
partial pressures of ethanol (A) and water (B) in three distillation
70 3.4 setups using log temperature readings. The table also includes
activity coefficients for both components, derived from the
80 3.8 measured temperatures.

Table 4.7 Total Pressure, Xa and Ya values of ETOH-water

Table 4.4 The refractometry results for the third distillation setup Set-up Pt xA yA
reveal the ethanol-water ratio in the liquid product over time, 1 88281.5720 0.5960 0.7377504594
measured at five-minute intervals. The data shows that the
2 100024.6364 0.5965 0.625266305
ethanol content rises as the distillation process progresses. The
boiling point of the first drop is 81 degrees Celsius or 354.15 3 104603.3211 0.5972 0.6483697084
Kelvin.

Table 4.5 Feed, Distillate, and Waste Composition of the

Three Set-ups Table 4.7 shows the total pressures for ethanol (A) and water (B)
in the distillation process across three setups. The table also
presents calculated values of Xa and Ya for the ethanol-water
xF Tb D xD W xW solution at recorded temperatures.
F
(°C
)

1 500 0.5 78 35 0.5960 465 0.4928

2 500 0.5 79 37 0.5965 463 0.4923

3 500 0.5 81 38 0.5972 462 0.4920

Figure 4.1 Set-up 1 T-x-y Diagram of EtOH-Water Mixture

Table 4.5 Summarizes the distillate and bottoms compositions of

three distillation setups using overall material balance and
component balances, all with identical feed compositions.

Table 4.6 Saturated Vapor Pressure, Partial Pressure, and

Activity Coefficients of ETOH and Water for the various
set-ups
 2. What is relative volatility?
Relative volatility is a term used in distillation
to measure the difference in volatility between two
substances in a mixture. It is defined as the ratio of the
vapor pressures of the two substances. In other words, it
is a measure of the ease or difficulty of using distillation
to separate the more volatile components from the less
volatile components in a mixture. The greater the
difference in relative volatility between two substances,
the easier it is to separate them by distillation.
Figure 4.2 Set-up 2 T-x-y Diagram of EtOH-Water Mixture Furthermore, Relative volatility is also expressed as:
𝑃*𝐴
𝑃 𝑃*𝐴
α𝐴𝐵 = 𝑃*𝐵 = 𝑃*𝐵
𝑃

Thus, this equation is the ratio of the K value

for the volatility of component A over B. It is usually
used in absorption and separation processes since it is
easier than separating components efficiently. However,
this equation will still depend only on pressure.

3. Derive the equations for enriching section, stripping

section and feed line.

Figure 4.3 Set-up 3 T-x-y Diagram of EtOH-Water Mixture

Figures 4.1 to 4.3 depict T-xy diagrams for ethanol-water

mixtures in three distillation setups. Each diagram shows phase
behaviors under various conditions. The horizontal axis
represents mixture compositions, and the vertical axis represents
temperature. The diagrams reveal when phase changes occur and
how ethanol and water separate in constant intervals.

5 QUESTIONS OMB: 𝑉𝑛+1 = 𝐿𝑛 + 𝐷

1. Discuss the different distillation methods? CMB: 𝑦𝑛+1𝑉𝑛+1 = 𝑥𝑛𝐿𝑛 + 𝑥𝐷𝐷
There are 5 different distillation methods,
namely; Simple distillation, Fractional distillation, Thus, we have:
Steam distillation, Vacuum distillation, and Continuous (𝐿𝑛 + 𝐷 )𝑌𝑛+1 = 𝑥𝑛𝐿𝑛 + + 𝑥𝐷𝐷
distillation. These distillations are determined on which
Under constant molal overflow assumption:
fits the solution. Simple distillation is used when two
substances have a temperature difference of 25C. While 𝐿1 = 𝐿2 − ... 𝐿𝑛−1 = 𝐿𝑛 = 𝐿𝑛+1 = 𝐿 = 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡
Fractional Distillation is used to separate two elements 𝑉1 = 𝑉2 − ... 𝑉𝑛−1 = 𝑉𝑛 = 𝑉𝑛+1 = 𝑉 = 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡
with very close boiling points, it uses a three-way
adapter to enable purification. Steam Distillation is a Subscripts can be dropped and equation can be
method that uses steam to distill temperature-sensitive simplified as:
materials, then condense and collect. Vacuum 𝑅 1
𝑌𝑛+1 = 𝑥𝑛 + 𝑥𝐷
Distillation will be an ideal method when separating 𝑅+1 (𝑅+1)
𝑅 1
liquids with very high boiling points and Continuous 𝑌𝑛+1 = 𝑥 + 𝑥𝐷
𝑅+1 (𝑅+1)
distillation is used for large scale production of a single
product.
 operating lines are L/V = 1.0 wherein the slope indicates
that the relationship between each plate would be equal
(y=x). If the entire reflux has been obtained, t minimum
quantity of theoretical plates are needed. Since, the
lowest values of reflux are which separation may be
achieved with an infinite number of plates (Minimum
Reflux Ratio) wherein this can be expressed as ratio (R
min). Furthermore, a separation can be accomplished at
any reflux ratio since the number of theoretical plates
that are necessary is reduced if there will be a possibility
that there will be an increase in the reflux ratio.

OMB: 𝑉𝑚+1 = 𝐿𝑚 +W 5. A mixture of 100 kg mol which contains 60 mol%

CMB: 𝑦𝑚+1𝑉𝑛𝑚1 = 𝑥𝑚𝐿𝑚 + 𝑥𝑚𝑊 n-pentane and 40 mol% n-heptane is vaporized at 101.32
kPa under differential conditions until 40 kg mol are
distilled. Using equilibrium data:
Substitution and rearranging in the form of y=f(x), we a. What is the average composition of the total
obtain: vapor distilled and the composition of the
𝐿' 𝐵
𝑦𝑚+1 = ( 𝑉' )𝑥𝑚 − ( 𝑉' )𝑥𝐵 remaining liquid?

𝑥1
Substituting V’= L’ - B, stripping section equation is: 𝐿1 𝑑𝑥
𝑙𝑛 𝐿2
= ∫ 𝑦−𝑥
𝑥2
𝐿' 𝐵
𝑦 = ( 𝐿'−𝐵 )𝑥 − ( 𝐿'−𝐵 )𝑥𝐵 0.6
100 𝑑𝑥
𝑙𝑛 60
= ∫ 𝑦−𝑥
𝑥2
Feed Line 0.6
𝑑𝑥
0. 5105 = ∫ 𝑦−𝑥
𝑥2

b. If this same vaporization is done in an

equilibrium or flash distillation and 40 kg mol
are distilled, what is the composition of the
vapor distilled and of the remaining liquid?

6. Calculate the approximate minimum number of stages

for a binary system with relative volatility of 2.35,
fractionally distilled to yield compositions of 0.98 in the
distillate and 0.045 in the bottoms.
OMB: 𝐹𝑥𝐹 = 𝐷𝑥𝐷 + 𝑊𝑥𝑊
𝑞 = 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑙𝑖𝑞𝑢𝑖𝑑 𝑖𝑛 𝑓𝑒𝑒𝑑 Using Fenske Equation:
𝐿𝑚 = 𝐿𝑛 + 𝑞𝐹 𝑙𝑜𝑔
𝑥𝐷(1−𝑥𝑊)
𝑥𝑤(1−𝑥𝐷)

𝑉𝑛 = 𝑉𝑚 + (1 − 𝑞)𝐹 Number of Stages = 𝑙𝑜𝑔α

0.98(1−0.045)
𝑙𝑜𝑔 (1−0.98)(0.045)
CMB: 𝑦𝑚+1𝑉𝑚+1 = 𝑥𝑚𝐿𝑚 + 𝑥𝑚𝑊 Number of Stages = 𝑙𝑜𝑔(2.35)
𝑞 1
𝐹𝑒𝑒𝑑 𝑙𝑖𝑛𝑒 : 𝑦 = (𝑥) − (𝑥𝐹) Number of Stages = 8.13
𝑞−1 𝑞−1

7. A rectification column is fed 100 kg mol of a mixture of

4. Differentiate total and minimum reflux ratio.
50 mol% benzene and 50 mol% toluene at 101.32 kPa
abs pressure. The feed is liquid at the boiling point. The
The difference between total and minimum reflux ratio
distillate is to contain 90 mol% benzene and the bottoms
is that total reflux ratio occurs when liquid and vapor
10 mol% benzene, The reflux ratio is 4.521. Calculate
pass each other in a column without losing any products.
the kgmol/h distillate, kmoV/h bottoms, and the number
Wherein D=0 and R= L/D). With this, the slopes of
 of theoretical trays needed using the McCabe-Thiele N = 6 = n+1 = 5 theoretical trays + 1 reboiler
method.
n = 5 theoretical trays
𝐹=𝐷+𝐵
100 = D+B 6 CONCLUSION
𝐹𝑥𝐹 = 𝐷𝑥𝐷+𝐵𝑥𝐵
100(0.5) = D(0.90) + B(0.1)
Distillation involves the separation of constituents
within liquid mixtures by selective evaporation and
D= 50 kgmol/hr B = 50 kgmol/hr condensation. This method is applied for purifying liquids
and isolating various liquid blends. During distillation, the
Benzene-Toluene liquid is heated to its boiling point, and the resulting vapor
x y is condensed back into a liquid state. The distillation curves
observed in each trial displayed a consistent pattern with
0 0 slight variations, affirming the experiment's reproducibility.
Utilizing the average densities from multiple trials, an
0.1 0.21
overall distillation curve was constructed. Through batch
0.2 0.37 distillation, the ethanol concentration increased from 25%
to 95% over time, but further separation was constrained by
0.3 0.51 the azeotropic composition. The gradual decrease in
density, as measured by the pycnometer, indicated shifts in
0.4 0.64 the distillate's composition. To ensure the reliability of the
findings, the experiment was repeated in three trials. Up to
0.5 0.72
the azeotrope, ethanol-water mixtures exhibited ideal
0.6 0.79 behavior.

0.7 0.86
7 HAZARDS
0.8 0.91 ● The hazard of liquid spillage or vapor leakage from
the experimental apparatus, which could lead to
0.9 0.96 unintended consequences and safety issues.
● The potential hazard of exposure to flammable or
0.95 0.98
toxic vapors emanating from the distillate or the
1 1 boiling liquid.
● The risk of sustaining burns or scalds arising from
hot glassware, steam, or boiling liquids during the
experimental process.
● The possibility of glassware breakage resulting
from thermal stress, overpressure, or mishandling,
posing a threat to individuals in the vicinity.

8 WASTE DISPOSAL
In this experiment, ethanol and water were the
substances used. Ethanol and water do not require any
𝑥𝑑
𝑦 − 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 = =
0.9
= 0. 163 particular handling while being disposed of; they can
𝑅+1 4.52+1
simply be put into a sink. In instances where the denatured
alcohol-water solution is primarily water containing solid
residues, you can solidify the waste before disposal. This
can be achieved by incorporating absorbent materials such
as kitty litter or sawdust, allowing for solidification, and
then adhering to local regulations for proper disposal. In the
presence of neutralization, depending on the composition of
additives in the denatured alcohol, there may be an
opportunity to neutralize the solution prior to disposal.

9 APPENDIX

REFERENCES

Bravo, Jose L. and James K. Fair. “Distillation Columns.”

Chemical Engineering Progress January 1990: 19-29.

Humphrey, Jimmy L. “Separation Processes: Playing a

Critical Role.” Chemical Engineering Process October
1995.

Stephen Hall, in Branan's Rules of Thumb for Chemical

Engineers (Fifth Edition). (2012).
https://doi.org/10.1016/B978-0-12-387785-7.0 0003-7

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