3.

0 Results and Calculations

Result for calibration curve:
Sample Table For Preparation of Refractive Index Versus Composition:
Molar volume of ethanol= 17.13 mol/L
Molar volume of water = 55.49 mol/L

No of mol of
ethanol
0
0.01712622
0.03425244

No of mol of
water
0.55493895
7
0.49944506
1
0.44395116
5

0.051378661 0.38845727
0.33296337
0.068504881
4
0.27746947
0.085631101
8
0.22197558
0.102757321
3
0.16648168
0.119883542
7
0.11098779
0.137009762
1
0.08324084
0.145572872
4
0.05549389
0.154135982
6
0.02774694
0.162699092
8
0.171262202

Total
mole
0.554938
96
0.516571
28
0.478203
61
0.439835
93
0.401468
26
0.363100
58
0.324732
9
0.286365
23
0.247997
55
0.228813
72
0.209629
88
0.190446
04
0.171262
2

mole fraction
ethanol

mole fraction refractive

water
index

1.33299

0.033153644

0.966846356

1.33719

0.071627315

0.928372685

1.34328

0.116813241

0.883186759

1.34919

0.17063586

0.82936414

1.35423

0.235833006

0.764166994

1.35845

0.316436432

0.683563568

1.36096

0.418638611

0.581361389

1.36304

0.552464168

0.447535832

1.36358

0.636206932

0.363793068

1.36325

0.735276783

0.264723217

1.36273

0.854305462

0.145694538

1.36116

1.36096

Table 3.1

Xd =
Xb =
0.1706

refractive index vs. mole fraction of ethanol

12
10
8

y- data
Linear (y- data)

6
4
2
0

f(x) =
0 R =0.2
0

0.4

0.6

0.8

1.2

Graph 3.1 : refractive index against mole fraction of ethanol (calibration curve)

1) Calculation Molar Volume of Ethanol

From appendix E in manual,
Specific gravity of ethanol = 0.789
Specific gravity of water = 1.000.
Density of water = 1.000 g/mL.
3
Density of ethanol = 789 kg/ m

= 0.789 g/mL

Molecular weight (MW) of ethanol= 46.07g/mol

1 mol
Molar volume of ethanol = 46.07 g

0.789 g
1 mL

1000 mL
1L

=17.13 mol/L

2) Calculation Molar Volume of Water

Density of water = 1000kg/ m

= 1 g/mL
Molecular weight (MW) of water= 18.02 g/mol
1mol
Molar volume of water= 18.02 g

1g

X 1 mL

1000 mL
1L

3) Calculation of Mole Fraction

For this sample, second set of data is used.
For second set of data,
Volume of Ethanol = 1.0mL or 0.001 L
Volume of water

= 9.0mL or 0.009 L

Mole of ethanol = Molar Volume X Volume

17.13 mol
X 0.001 L
=
L
= 0.01712622 mole

=55.49 mol/L

Mole of water =

55.49 mol
X 0.009 L
L

= 0.499445061 mole
Mole of ethanol
Mole fraction of ethanol = Mole of ethanol + Mole of water
0.01712
= 0.01712+0.49941

Mole fraction of water

= 0.033153644
Mole of water
Mole of ethanol + Mole of water

0.49941
0.01712+ 0.49941

= 0.966846356
Calculation is repeated for all set of data.

Experiment 1 : Batch Distillation at Total Reflux

Heate
r

Distillate
Temp

Refractive
index

Bottom
Mole frac
(Xd)

Temp

Refractive
index

HETP
Mole frac
(Xb)

100

74.5

1.3562

0.20107

80.1

1.35585

0.19566

1120

80

79.8

1.35446

0.17419

73.3

1.36191

0.14306

1120

60

79.7

1.35356

0.16348

72.9

1.36225

0.08101

1120

40

79.8

1.35259

0.15312

72.5

1.36206

0.11568

1120

20

79.7

1.35187

0.14543 72.4
Table 3.2

1.36229

0.07371

1120

Taking mole fraction of distillate = 0.400394, mole fraction of bottom product = 0.108481, the no. of
theoretical plates can be determined from the X-Y equilibrium diagram for ethanol-water system at 1atm
from APPENDIX A.2.

HETP vs Power Supply

1150
1100
1050
1000
HETP(mm)

HETP

950
900
850
800
10

20

30

40

50

60

70

80

Power Supply (%)

Graph 3.2 HETP Vs Power Supply

90 100 110

Refractive index vs Mole Fraction

1.36
1.36
1.36
1.35
Refractive index

1.35

Distillate

1.35
1.35
1.35
0.15

0.16

0.17

0.18

0.19

Mole Fraction,X

Graph 3.3 Refractive index Vs Mole Fraction

0.2

0.21

Refractive index vs Mole Fraction

1.36
1.36
1.36
Refractive index

1.36

Bottom

1.36
1.35
1.35
0.06 0.08 0.1 0.12 0.14 0.16 0.18 0.2 0.22
Mole fraction,x

Graph 3.4 - Refractive index vs Mole Fraction

Sample Calculation For experiment 1:

To calculate HETP:
For this sample calculation, data for 100% heater power is used.
Height of column = 1120mm
HETP=

Height of column
Number of stages

HETP=

1120
1

HETP=1120 mm

#Repeat the calculations for all the data respective to the percentage heater power.

Experiment 2 : Batch Distillation at Constant Reflux

Results:

tem
time
p
0

76.1

10

75.3

20

75.3

30

75.3

40

75.3

Refracti
volu
ve
me
index
1.3609
4
11
1.3592
3
11
1.3593
7 10.75
1.3591
6
11
1.3593
7 12.5

Mole
frac
(Xd)
0.3157
94
0.2608
81
0.2653
77
0.2586
33
0.2653
77

Flow
rate
50/17
0s
50/21
4s
50/21
9s
60/26
4s
50/21
7s

tem
p

Refracti
ve
index

79.9 1.36224
80

1.36216

80.1 1.36208
80.1 1.36205
80.1

1.362

Mole
volum HET
frac
e
P
(Xb)
0.0828
112
31
6.5
0
0.0974
112
32 8.75
0
0.1120
112
32 10.5
0
0.1175
112
07
9.5
0
0.1266
112
32
7.2
0

1/y

4.2
53
6.1
1
6.5
25
7.0
87
7.2
49

50

75.5

1.3599
1 12.75

60

75.5

1.3601

11.5

0.2827
18
0.2888
19

Calculation for Experiment 2:

To calculate XD /(R+1) :
In this sample, data for time interval=0 is used
For Y-intercept value,( XD /(R+1) )
t=00

X D=0.315794
R=1
X D ( R+1)
0.315794 ( 1+ 1 )
0.315794 2

0.157897

50/22
1s
50/24
3s

80.2 1.36199
80.2 1.36186

0.1284
57
0.1521
83

10.5
13

112 6.4
0
54
112 7.3
0
69

Then, to calculate HETP at time 0,

t =0
Based on graph given in the appendices,

number of stages=1

Height of column= 1120mm

HETP=

Height of co lumn
Number of stages

HETP=

1120 mm
1

HETP=1120 mm
# Repeat the calculation for others data using this step to calculate HETP

HETP
1200
1000
800
HETP(mm)

600

HETP

400
200
0
0

10

20

30

40

50

60

70

Time

Graph 3.5 - graph number of theoretical stage, HETP against time interval

For Mass Balance Calculations:

Initial Conditions:
Reboiler volume

= 15.0 L

Reboiler composition = 0.082831 (value taken from XB at t=0min table 3.3)

Final Conditions:
Reboiler volume

= 13.0L

Reboiler composition = 0.152183 ( value taken from XB at t=60min Table 3.3)

Distillate volume

= 1.5 L

Distillate composition = 0.288819 (value taken from XD at t=60 min Table 3.3)

Around 0.14645 L of sample from the reboiler has been withdraw in order to test the refractive index.
Final reboiler volume
= initial reboiler volume final distillate volume loss of volume due to sample testing
= 15.0L 1.5L 0.14645L
= 13.353 L

Refractive index vs Mole Fraction

1.36
1.36
1.36
1.36
Refractive index

1.36

Distillate

1.36
1.36
1.36
0.25 0.26 0.27 0.28 0.29

0.3

Mole Fraction,Xd

0.31 0.32

Graph 3.6 refractive vs mole fraction

Refractive index vs Mole Fraction

1.36
1.36
1.36
1.36
Refractive index

Bottom

1.36
1.36
1.36
1.36
0.05

0.07

0.09

0.11

0.13

Mole Fraction,Xb

Graph 3.7 Refractive index vs Mole fraction

0.15

0.17

1/(Y-X) vs Xb
8
7
6
5
1/(y-X)

4
3
2
1
0
0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

Xb

Graph 3.8 : Graph

1
y x

versus XB for Different Time Interval to Determine the Area under the Curve

To calculate Area Under the Curve:

Area of a Complete big box= 0.02 X 1 =0.02
Approximate Number of the boxes under the curve= 20.5

Total area under the curve= 20.5 (0.02) = 0.41

According to Rayleighs equation as in the manual:
n0

x0

dx
n0
=
=ln
dn
n1
n1 n
x1 y x
dx
y x
x0

x1

exp
n0
n 1=
Where t0= initial condition,
t1= final condition,
x= bottom composition,
y= top composition,
n= total number of moles of ethanol in the reboiler.
Calculation of Theoretical Value of Amount of Ethanol Left in the Reboiler
ln

n0
ln
=area under the curve of Graph3.8 Graph
n1

n0
dx
=
n1
y x

1
y x

versus XB for Different Time Interval)

n1=

n0
exp ( area under the graph)

n0 ethanol=

17.12 mol ethanol

( 0.3)(15.0 L mixture)=77.04 mol ethanol
L
n0 water =

n1=

55.49 mol water

( 0.7 )( 15.0 L mixture )
= 582.645 mol water
L

77.04 mol ethanol

=64.74 mol
exp(0.174)

Mole Fraction of ethanol VS Time

0.2
0.15
Xb

0.1

Xb

0.05
0
0

10

20

30

40

50

60

70

Time

Graph 3.9 : Graph mole fraction of ethanol left in reboiler against time

Performing a Mass Balance Calculation on the Distillation Column and Compare with the
Experimental Results
Total mass balance formula

i)

F o = D1 + B 1
F0

total mole in feed

D1

total mole in distillate

B1

total mole in reboiler

ii)

Component mass balance formula

F0 x0 = D1 xD1 + B1 xB1

x0

mole fraction of ethanol in feed

xD1

mole fraction of ethanol in distillate

xB1

mole fraction of ethanol in reboiler

Initial Conditions:
Reboiler volume

= 15.0 L

Reboiler composition = 0.082831

Final Conditions:
Reboiler volume

= 13.0L

Reboiler composition = 0.152183

Distillate volume

= 1.5L

Distillate composition = 0.288819

Substituting the final value of the composition of the distillate and bottom produce into the mass balance
equation,
15(xo)=13.0(0.152183)+1.5(0.288819)
X0

13.0 ( 0.152183 ) +1.5 ( 0.288819 )

15

= 0.161 (Theoretical value for the initial value of mole fraction of ethanol)
Experimental value for the initial value of mole fraction of ethanol= 0.126

Percentage error =

Experimental ValueTheoretical Value

X 100
Theoretical Value

|0.1521830.161
| X 100%
0.161

=5.47%