REG # 2017-PE-21 DEPT OF POLYMER &PROCESS ENGG

Lab Report
Course Title: Mass Transfer (PPE-205L)
Experiment No: 1
Title: Use of the refractometer to find out the composition of mixture obtained from Batch
Distillation Column.

Name: Mian Husnain Iqbal

Roll Number: 2017-PE-21

Submitted to: Miss Fazila

Submitted date: 26 FEB 2019

Semester: 04
Group no: 04

Department of Polymer and Process Engineering,

University of Engineering and Technology Lahore

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REG # 2017-PE-21 DEPT OF POLYMER &PROCESS ENGG

Contents

1.1. Objective..............................................................................................................................................3
1.2. Introduction..........................................................................................................................................3
.................................................................................................................................................................3
1.2.1. Batch Distillation...........................................................................................................................3
1.2.2. Refractive index.............................................................................................................................4
1.3. Apparatus required...............................................................................................................................5
1.4. Chemicals.............................................................................................................................................5
1.5. Procedure of the experiment.................................................................................................................5
1.5.1. Procedures for the standard composition curve..............................................................................5
1.5.2. Procedure on the batch distillator...................................................................................................5
1.6. Calculations:.........................................................................................................................................5
1.6.1. Standard curve formation...............................................................................................................5
1.7. References............................................................................................................................................7

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REG # 2017-PE-21 DEPT OF POLYMER &PROCESS ENGG

1.1. Objective
Use of the refractometer to find out the composition of mixture obtained from Batch Distillation
Column.

1.2. Introduction
Batch distillation refers to the use of distillation in batches, meaning that a mixture is distilled to
separate it into its component fractions before the distillation still is again charged with more mixture
and the process is repeated. This is in contrast with continuous distillation where the feedstock is
added and the distillate drawn off without interruption. Batch distillation has always been an
important part of the production of seasonal, or low capacity and high-purity chemicals. It is a very
frequent separation process in the pharmaceutical industry.

Figure 2.2 batch distillation apparatus

1.2.1. Batch Distillation

Batch distillation is a type of distillation in which the feed is not continuously added rather it is
added once. The main components of a distillation column are given by

 A vertical shell where separation of liquid components is performed.

 Column internals e.g. trays/plates and/or packings which are used to enhance component
separations.

 A reboiler to provide the necessary vaporization for the distillation process.

 A condenser to cool and condense the vapour leaving the top of the column.

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 A reflux drum to hold the condensed vapour from the top of the column so that liquid
(reflux) can be recycled back.

Figure 1.2 schematic of batch reactor

1.2.2. Refractive index

For the system, Ethanol/ Water, mixtures of known concentration can be made up and their
refractive indexes measured. The refractometer measures the critical angle of liquid undertest
and each concentration will show a different critical angle. Beyond the critical angle is darkness
and refractometers are calibrated along this light/dark boundary.

Figure 2.3 refractometer

Standard for measuring refractive index (R.I):

First, we make a mixture of Ethanol/Water of known concentration then plot the concentration
versus refractive index (R.I). we get a standardize curve from which we can find the un known
concentration of a mixture by knowing its refractive index from refractometer.

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1.3. Apparatus required

1. Batch distillation apparatus

2. Hand held refractometer

3. Measuring cylinders

1.4. Chemicals
1. Distilled water

2. Ethanol

1.5. Procedure of the experiment

1.5.1. Procedures for the standard composition curve

 First six solutions of known concentrations of ethanol and water are prepared.

 The concentrations are 0,20,40,60,80,100% of ethanol.

 Then their refractive indexes are measured by refractometer.

 Then the graph was plotted between percentage composition and the refractive index.

 The graph will give us the standard curve.

1.5.2. Procedure on the batch distillator

 The reboiler of batch distillation column is fed with the 1:1 of ethanol and water.
 Then we run it for different reflux rates and the refractive index was measured for every
reflux product.
 Then the fractions are calculated.
 Then theoretical number of trays are calculated.
 Then efficiency of the batch distillation column was calculated.
 for accurate results.

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1.6. Calculations:

1.6.1. Standard curve formation

 Calculated data from experiment for the six solutions

Refractive index Vs ethanol percentage

1.37
water %1.36 Ethanol
f(x) = 0.04 x +refractive
1.33 index
1.35
% We obtain this equation from graph we
refractive index

100%
1.34 0% 1.327 get value of y (refractive index from
1.33 refractometer) by putting its value of x
80%
1.32 20% 1.334 (% ethanol) is obtained.
1.31
60% 40% 1.346 Y= 0.0387x + 1.3285 …… (1)
1.3
0% 20% 40% 60% 80% 100% 120%
40% 60% 1.356
ethanol percentage

20% 80% 1.361

0% 100% 1.363
Graph 1.1 standard curve
Table 1.1 standard curve data

Percentage of ethanol can also be find by two point formula.

Up stream Down stream

 
Flux Temperature Refractive Composition Temperature Refractive Composition
(oC) index index
  XA XB (oC) XA XB
0.287 0.687
0 72.8 1.357 0.7125 76.7 1.356 0.3125
5 5
0.387 0.637
+2, -8 73.6 1.353 0.6125 76.9 1.354 0.3625
5 5

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0.412 0.662
+4, -6 73.8 1.352 0.5875 77.1 1.355 0.3375
5 5
0.312 0.712
+6, -4 75.4 1.356 0.6875 78.5 1.357 0.2875
5 5
0.287 0.612
+8, -2 75.5 1.357 0.7125 78.6 1.353 0.3875
5 5

The data for the up and the down streams for different flux ratios are given in the table 1.2.

Here XA= mole fraction of water

XB= mole fraction of ethanol

Both of are calculated by the two point formula or by using equation 1.

Number of theoretical plates:

The number of theoretical plates can be calculated by using the Fenske’s equation

1.7. References
1. http://1.bp.blogspot.com/_dpZfkyjb7QI/SZAe03s37AI/AAAAAAAAAbM/pfaW2kWrE
Ug/s400/New+Picture.png
2. https://www.academia.edu/11570902/Batch_Distillation_Column
3. http://www.separationprocesses.com/Distillation/DT_Chp05.html
4. http://www.rccostello.com/distil/distiltyp.htm