4.1.

1 Calibration graph
To determine the points on the coexistence curve and to plot the calibration graph, the method
used was refractive index method (Letcher et al., 2003). The specific amount of deep eutectic
solvent and n-heptane were weighed and added in sample bottle. Toluene was added by using
burette to the weighed mixture in the sample bottle and amount of toluene added was also
weighed. The sample mixture of three components was mixed thoroughly, until it forms
homogenous clear solution. Then, the refractive index of the sample considered was measured
using the ATAGO RX-7000i Automatic Digital Refractometer. The measured values of
refractive indices for the respective mole fraction of components for the extract and raffinate
phases were tabulated in Table 4.6 and Table 4.7 respectively.

Table 4.6 Measured values of refractive index at 25 0C for the respective mole fractions of
components for the extract phase
Measured wt Mole fraction
Empty RI at
S.NO Wt. of Wt. of Wt. of
Wt. X DES X tol X hep 25 0C
DES tol Hep
1 22.1299 5.1421 0.1371 0.0209 0.962 0.034 0.005 1.55855
2 22.2486 4.9769 0.2021 0.0209 0.945 0.050 0.005 1.55821
3 22.312 4.8971 0.2698 0.0215 0.928 0.067 0.005 1.55784
4 24.5959 4.8588 0.3813 0.0212 0.902 0.093 0.005 1.55719
5 25.9493 4.8229 0.3540 0.0230 0.907 0.088 0.005 1.55729
6 26.125 4.7355 0.4599 0.0288 0.881 0.112 0.006 1.5567
7 25.6405 4.3906 0.3731 0.0253 0.894 0.100 0.006 1.55694
8 26.135 4.6890 0.4819 0.0289 0.875 0.118 0.007 1.55652
9 25.9491 4.6193 0.4908 0.0310 0.871 0.122 0.007 1.55645
10 24.5689 4.6412 0.5480 0.0304 0.860 0.133 0.007 1.55619
11 22.2484 4.5953 0.5816 0.0390 0.850 0.141 0.009 1.55592
12 24.8253 4.5249 0.5870 0.0309 0.848 0.145 0.007 1.55583
13 25.9743 4.4428 0.8581 0 0.798 0.202 0.000 1.55497
14 25.4985 4.3801 0.9395 0 0.780 0.220 0.000 1.55415
15 24.5682 3.8680 1.5213 0 0.659 0.341 0.000 1.55259
 1.559

1.558

1.557
REFRACTIVE INDEX

1.556
y = -0.0192x + 1.5589
1.555 R = 0.9845

1.554

1.553

1.552

1.551
0.0000 0.0500 0.1000 0.1500 0.2000 0.2500 0.3000 0.3500 0.4000
XTOL

Figure 4.7 Calibration graph for the extract phase

Table 4.7 Measured values of refractive index at 25 0C for the respective mole fractions of
components for the raffinate phase
Measured wt Mole fraction
Empty RI at
S.NO Wt. of Wt. of Wt. of
Wt. X DES X tol X hep 25 0C
DES tol Hep
1 26.135 0.0000 0.0000 10.0000 0.000 0.000 1.000 1.3825
2 24.5689 0.0000 1.3508 8.6491 0.000 0.145 0.855 1.396
3 22.2484 0.0000 2.5858 7.4141 0.000 0.275 0.725 1.40884
4 24.5959 0.0000 3.7747 6.2252 0.000 0.397 0.603 1.42161
5 25.9493 0.0000 5.1115 4.8884 0.000 0.532 0.468 1.43639
6 26.125 0.0000 6.1553 3.8446 0.000 0.635 0.365 1.44824
7 25.9743 0.0000 6.8342 3.1657 0.000 0.701 0.299 1.45607
8 24.5682 0.0000 7.8843 2.1156 0.000 0.802 0.198 1.46838
9 23.5264 0.0000 8.7638 1.2361 0.000 0.885 0.115 1.47885
10 25.6235 0.0000 10.0000 0.0000 0.000 1.000 0.000 1.49382

Hence, the calibration plot was plotted between refractive index readings obtained for
samples considered and the mole fraction of each component was shown in Figure 4.7 and
Figure 4.8 for the extract and raffinate phases respectively.
 1.5075

1.4875

1.4675
REFRACTIVE INDEX

1.4475
y = 0.1113x + 1.3792
R = 0.997
1.4275

1.4075

1.3875

1.3675
0 0.2 0.4 0.6 0.8 1 1.2
XTOL

Figure 4.8 Calibration graph for the Raffinate phase