CH 3520: Heat and Mass Transfer Laboratory, January-May 2015

Title of the experiment: Batch Distillation

Date of experiment:

20/01/2015

Date of Report:

26/01/2015

For Instructors use only:

No Division

Max. Marks

Introduction / background theory

Experimental details; materials and methods

Experimental observations; data

10

Sample calculations

30

Error analysis

Results, discussion and conclusions

Suggestions for improvement

Marks

40

References
Overall formatting

20

Total

100

Batch and group number: Batch B- Group Number 13

Name

Roll Number

RishabhSethiya

CH12B055

S DheerajSharavan

CH12B056

S Gokulakannan

CH12B057

Sanket Wani

CH12B059

Marks:

100

CH 3520: Heat and Mass Transfer Laboratory, January-May 2015

INTRODUCTION / BACKGROUND THEORY

Simple distillation, also known as Rayleigh distillation or differential distillation is the most
elementary example of batch distillation. In this distillation system, the vapour is removed from the
still during a particular time interval and is condensed in the condenser. The more volatile
component is richer in the vapour than in the liquid remaining in the still. Over time, the liquid
remaining in the still begins to experience a decline in the concentration of the more volatile
component, while the distillate collected in the condenser becomes progressively more enriched in
the more volatile component.
In the case of differential distillation, the vapour at any time is in equilibrium with the liquid
from which it rises but changes continuously in the composition. Thus, the mathematical approach
used must be differential. Assume that L mol of liquid in the still of composition x mol fraction A
and that an amount dDmol of distillate is vaporized, of mol fraction y in equilibrium with the
liquid.
The rate of depletion of liquid is equal to the rate of distillate output. The instantaneous rate of
depletion of a component in the liquid is therefore, In - out = accumulation.
Taking balance on more volatile component, rearranging and integrating, we get the following
form which is called the Rayleighs Equation,

(1)

where, F = moles of feed of composition x F , W= moles of residual composition xW, W and

xwcan be obtained by material balance.
=+
(2)
= +
(3)
The integral in equation 1 can be solved analytically (provided the relationship between y* and
x is available) or graphically (calculating the area under the curve for the plot of 1/(y*-x) vs x.
2

EXPERIMENTAL DETAILS; MATERIALS AND METHODS

A simple experimental setup is shown in figure 1.

Figure 1: Experimental Setup for Batch/Simple Distillation.

2

CH 3520: Heat and Mass Transfer Laboratory, January-May 2015

A similar setup was used in the laboratory.

1.

2.
3.
4.
5.
6.
3

Procedure:
A calibration chart with refractive index of liquid mixtures of ethanol water system along Y
axis and mole fraction(and volume fraction) of ethanol in the mixture along X axis is
prepared using 11 data points.
Known volume of the ethanol water mixture is transferred to the round bottomed flask and
heated. A constant heat input is maintained.
Water is admitted to the condenser and the heater is switched on.
Observe the first drop of distillate when the temperature reaches between the boiling points
of water and ethanol.
Collect and measure the volume samples from the residue as well as the distillate flasks as a
function of rise in temperature .
Composition of residue and distillate is found out using calibration chart.
EXPERIMENTAL OBSERVATIONS; DATA
Density of water : 1 gm/cm3
Density of ethanol : 0.78 gm/cm3
Molecular weight of water: 18 g/mol
Molecular weight of ethanol: 46 g/mol

Table 1: Calibration table ( volume fraction vs refractive index)

Mole fraction
Volume fraction of ethanol Refractive Index
ethanol
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1

1.33298
1.33809
1.3536
1.35906
1.36142
1.36196
1.36224
1.36256
1.36259
1.36261
1.3627

of

0
0.032800673
0.070894769
0.115676151
0.169075145
0.233844104
0.314047122
0.415947181
0.54972592
0.733116732
1

CH 3520: Heat and Mass Transfer Laboratory, January-May 2015

Refractive index of mixtures

1.365
1.36
1.355
1.35
Refractive Index
1.345
1.34
1.335
1.33

refractive index of
mixtures

0.5

1.5

volume fraction of ethanol

Figure 2: Refractive index vs volume fraction of ethanol

Refractive index of mixtures

1.365
1.36
1.355
refractive 1.35
index
1.345
molefraction of
ethanol

1.34
1.335
1.33
0

0.5

1.5

molefraction of ethanol

Figure 3: Refractive index vs mole fraction of ethanol

SAMPLE CALCULATIONS

Table 2: Estimation of mole fractions of ethanol in residue and distillate

y*(mole
Refractive Index of
X(mole fraction of
Refractive
fraction
Residue
residue)
index of distillate
distillate)
1.3423
1.34263
1.34656
1.34234
1.34696
1.33956
1.34182

0.032632
0.0337789
0.0485778
0.0327703
0.0502199
0.0235819
0.030987

1.36247
1.36263
1.3623
1.36174
1.36214
1.36135
1.36116
4

of

0.180742
0.185683
0.176844
0.163286
0.172044
0.155991
0.152766

CH 3520: Heat and Mass Transfer Laboratory, January-May 2015

1.34642
1.33819

0.0480097
0.0193398

1.36149
1.36203

Table3: Estimation of RHS of Rayleighs Equation

Delta x
1/(y*-x)
6.751739
6.583101
7.796286
7.661913
8.208556
7.552351
8.211596
9.050896
6.660663

Integral
(1/(y*x))*(delta
x)

0.001147
0.014799
0.01581
0.01745
0.02664
0.007405
0.017023
0.02867
Total Integral

0.007744
0.097423
0.123259
0.1337
0.218676
0.055925
0.139786
0.259489
1.036

Table 4: Estimation of LHS

Moles = (density *volume)/molecular weight
Mole fraction of A = (moles of A)/(total moles )
Feed of ethanol
Feed of water
Total feed

3.391304
16.66667
20.05797

Table 5: Estimation of total moles in distillate

7.6064
0.38359
7.99

Moles of
water
Moles of
ethanol
Total moles

LHS :
ln(F/D)= 0.92

ERROR ANALYSIS
Error % =abs ((LHS-RHS)/(LHS))
Where LHS =ln(F/D)
RHS = Integral ((1/(y*-x)*delta x)
Error % = (1.036-0.92)/0.92 *100 =12.6%
5

0.158496
0.169475

CH 3520: Heat and Mass Transfer Laboratory, January-May 2015

RESULTS, DISCUSSION AND CONCLUSION

1. When we put our recorded and calculated values in the Rayleigh equation, the LHS
and RHS were found to be approximately equal.
2. Calibration chart was prepared for ethanol-water binary mixture. Refractive index
increases with increase in mole fraction till a point after which it stabilizes to the value
of refractive index of pure ethanol. Similar behaviour was observed in the Refractive
index vs Volume fraction graph. So we can conclude that the rate of separation isnt
appreciable at higher mole fractions, and that complete separation isnt feasible. This
isnt so in the case of continuous distillation, where there isnt any saturation and
complete separation is possible
3. One of the readings of the refractive index was ignored because it was an outlier. It
was uncharacteristically low compared to the adjacent values so we didnt consider it
in order to maintain the uniformity of values recorded.
4. The Rayleigh equation was verified for a binary mixture of ethanol and water using
simple distillation with an error of 12.6%.
5. Difference between the boiling temperatures of components of mixtures should be
considerable. Here boiling point of ethanol = 77 Degree Celsius and boiling point of
water =100 degree Celsius.

SUGGESTIONS
1. Take adequate amount of mixture feed so that temperature sensor remains dipped in
the solution throughout the experiment. When we performed the experiment, halfway
through it, the sensor was above the solution. So we had to complete the experiment
by measuring the temperature manually using a thermometer. This caused some of the
error.
2. While taking sample solution for measuring the refractive index, we took more
amount than optimally required as we had to do it manually using a pipette. If a micropipette was provided, we can increase the accuracy of the experiment.
3. Constant heat flux should be provided for the distillation of the binary mixture of
ethanol and water.

REFERENCES
[1] Robert E. Treybal, Mass-Transfer Operations, Third Edition, Tata McGraw-Hill, 2012
[2] CH3030 Applications of mass transfer class notes.
[3] Seader and Henley, Separation process principles, 2nd edtion