Transcript Fischer Esterification

Fischer Esterification
Maria Victoria Silva Elipe
Fischer Esterification Reaction
Detailed Methodology
•
•
•
•
•
•
•
•
1.8mL MeOH + 0.2mL CD3OD. The CD3OD is to lock in methanol so easy for the shimming
and aligning of the signals over time.
2mL AcOH + 10uL H2SO4.
I took 300 uL of the MeOH+CD3OD and added with a syringe in the outer chamber which is
wider and help shimming because there is more volume there and that’s why I need some
CD3OD.
I took 300 uL of the AcOH+H2SO4 and added in the inner chamber with a syringe with long
needle to make sure the liquid reach the bottom of the tube (if the liquid is viscose it is not
easy to put all the liquid down but a syringe with very long needle helps because my long
needles reach the bottom of the tube-I avoid to shake the tube specially before mixing for
precaution).
I tune and shim and take spectrum.
I take the tube out and lift the inner tube enough to mix the liquids from both chambers
but now I don’t remove the inner tube, just lift it enough for the mixing.
I put the sample inside the magnet and I shim again to make sure no signal degradation
and take spectra over time. Sometimes I may do autoshiming to make sure no degradation
of shimming occurs during time due to changes on pH and concentration during the
reaction.
I use Mnova software to do all the analysis of the reaction including calculating
concentrations overtime.
C' = B+F*exp(-t*G)
B=6.224; F=3.478; G=0.6907;
Error: 0.08679
C1' = B+F*exp(-t*G)
B=4.015; F=-3.735; G=0.7729;
Error: 0.02697
#
X(I)
Y(X)
Y'(X)
Y1(X)
Model
ARR_DATA(I)
[t(hr)]
Concentration(3.459,3.255)
1
0
11.11
9.702
-0.064
0.279
2
0.17
8.424
9.317
0.688
0.739
3
0.35
8.569
8.955
1.324
1.165
4
0.5
8.357
8.686
1.693
1.477
5
0.67
8.156
8.414
1.951
1.789
6
0.82
7.996
8.198
2.183
2.033
7
0.98
7.86
7.992
2.381
2.263
8
1.13
7.732
7.818
2.525
2.455
B+F*exp(-x*G)
B= 6.22437
F= 3.47756
Y1'(X)
B+F*exp(-x*G)
Concentration(3.652,3.592)
G= 0.690669
B= 4.01451
F= -3.73507
G= 0.772858
9
1.3
7.623
7.641
2.66
2.647
10
1.45
7.546
7.502
2.804
2.797
11
1.63
7.448
7.352
2.916
2.955
12
1.77
7.353
7.248
3.016
3.063
13
1.93
7.248
7.141
3.105
3.174
14
2.08
7.167
7.051
3.186
3.266
15
2.25
7.095
6.96
3.264
3.358
16
2.4
7.046
6.887
3.34
3.43
17
2.57
6.983
6.814
3.4
3.502
18
2.72
6.925
6.756
3.459
3.558
19
2.88
6.862
6.7
3.508
3.611
20
3.03
6.806
6.653
3.558
3.655
21
3.2
6.741
6.606
3.603
3.7
22
3.35
6.692
6.568
3.649
3.734
23
3.52
6.64
6.53
3.692
3.769
24
3.67
6.591
6.5
3.734
3.795
25
3.83
6.538
6.471
3.774
3.821
26
3.98
6.492
6.447
3.812
3.842
27
4.15
6.46
6.422
3.847
3.863
28
4.38
6.389
6.393
3.894
3.888
29
4.53
6.351
6.377
3.924
3.902
30
4.7
6.313
6.36
3.951
3.916
31
4.85
6.267
6.346
3.978
3.927
32
5.02
6.239
6.333
4.004
3.937
33
5.17
6.2
6.322
4.03
3.946
34
5.33
6.164
6.312
4.051
3.954
35
5.48
6.128
6.303
4.074
3.96
36
5.65
6.091
6.295
4.089
3.967
37
5.8
6.059
6.288
4.108
3.972