4 Case Study PDF

Case Study
GC analysis
Enzymatic trans-esterification of Ethyl Butyrate (EB) and
Butanol (BUT) in solvent hexane
Case Study
GC analysis
Ethyl Butyrate (EB) + Butanol (BUT)

Butyl Butyrate (BB) + ethanol (ETH)
Case Study
GC analysis
CH3CH2CH2COOCH2CH3 + C4H9OH
CH3CH2CH2COOC4H9 + CH2CH3OH

Case Study
GC analysis
CH3CH2CH2COOCH2CH3 + C4H9OH
CH3CH2CH2COOC4H9 + CH2CH3OH
116 74 144 46

Case Study
GC analysis

Case Study
GC analysis
Reaction volume = 1 L
???????? Timee va variation
at o oof
conversion and concentration

Case Study
GC analysis
Timee variation
va at o ofo conversion
co ve s o and
a d
concentration Time (min)
0
15
30
60
120
240
Ethyl Butyrate (EB) + Butanol (BUT) 500
Case Study
GC analysis
Timee variation
co ve s o and
a d
concentration
1 ml sample is taken for analysis in
sampling vials at different time
interval, 0.1 μL sample is injected in GC
equipped with capillary column

Case Study
GC analysis with FID
Timee variation
co ve s o and
a d
concentration
1 ml sample is taken for analysis in
sampling vials at different time
interval, 0.1 μL sample is injected in GC
equipped with capillary column & FID

Sample and stationery phase
Sample Classification
Gas Chromatography
Fig: Schematic Representation of gas chromatography

Gas Chromatography
Fig: Pictorial Representation of gas chromatography

GC with capillary column Sample 500 min
1 ml sample is taken for analysis in sampling vials at different
time interval,
interval 0.1
0 1 μL sample is injected in GC equipped with
capillary column & FID
Time (min)
0
15
30
60
120
240
500

1 ml sample is taken for analysis in sampling vials at different
time interval,
interval 0.1
0 1 μL sample is injected in GC equipped with
capillary column & FID
Time (min)
0
15
30
60
120
240
500

Split less injection

Gas Chromatography
Injection port
1 ~ 700
Split injection 1 is to 50

High temp
High mobile gas flow

Split injection 1 is to 50 Optimum temp
Optimum flow rate

Split injection 1 is to 50 Optimum temp
Optimum flow rate

GC with capillary column
Optimum temp
O ti
Optimum flow
fl rate
t
Pure Ethyl Butyrate (EB)

Optimum temp
O ti
Optimum flow
fl rate
t
Pure Butanol (BUT)

Optimum temp
O ti
Optimum flow
fl rate
t
Pure Butyl Butyrate (BB)

GC with capillary column Optimum temp
Optimum flow rate
Pure ethanol (ETH)


Area (sec.volt)
Time (min) EB BUT BB ETH
0
15
30
60
120
240
500 25227 27894 24105 8676
Area (sec.volt)
0 45203 49983 0 0
15
30
60
120
240
500 25227 27894 24105 8676
Area (sec.volt)
0 45203 49983 0 0
15 36638 40512 1895 682
30
60
120
240
500 25227 27894 24105 8676
Area (sec.volt)
0 45203 49983 0 0
15 36638 40512 1895 682
30 47670 52710 5708 2054
60 46519 51438 12876 4635
120 31636 34982 14601 5255
240 22093 24429 15053 5418
500 25227 27894 24105 8676
Area (sec.volt)
0 45203 49983 0 0
15 36638 40512 1895 682
30 47670 52710 5708 2054
60 46519 51438 12876 4635
120 31636 34982 14601 5255
240 22093 24429 15053 5418
500 25227 27894 24105 8676
60000
50000
40000
EB
30000 BUT
BB
20000
ETH
10000
0
0 100 200 300 400 500 600
Gas Chromatography
Injection port
Case 1
C 1 500 511
Case 2 1.1 50 51.1
10 0.196
1 ~ 700
Gas Chromatography
Internal stander
Injection port
Case 1
C 1 500 511
Case 2 1.1 50 51.1
10 0.196
1 ~ 700
Internal stander
Split injection 1 is to 50 granyl butyrate

Area (sec.volt)
Time (min) EB BUT BB ETH GB
0 45203 49983 0 0 6079 GB 3 mg/ml
15 36638 40512 1895 682 5243
30 47670 52710 5708 2054 7362
60 46519 51438 12876 4635 8402
120 31636 34982 14601 5255 6688
240 22093 24429 15053 5418 5480
500 25227 27894 24105 8676 7410
Area (sec.volt)
Time (min) EB BUT BB ETH GB
0 45203 49983 0 0 6079 GB 3 mg/ml
15 36638 40512 1895 682 5243
30 47670 52710 5708 2054 7362
60 46519 51438 12876 4635 8402
120 31636 34982 14601 5255 6688
240 22093 24429 15053 5418 5480
500 25227 27894 24105 8676 7410
AR
Time (min) EB/GB BUT/GB BB/GB ETH/GB
0 7.44 8.22 0.00 0.00
15 6.99 7.73 0.36 0.13
30 6 48
6.48 7 16
7.16 0 78
0.78 0 28
0.28
60 5.54 6.12 1.53 0.55
120 4.73 5.23 2.18 0.79
240 4.03 4.46 2.75 0.99
500 3.40 3.76 3.25 1.17
9.00
8.00
7.00
6.00
EB/GB
5.00
BUT/GB
4.00
BB/GB
3.00
ETH/GB
2.00
1.00
0.00
0 100 200 300 400 500 600
AR
0 7.44 8.22 0.00 0.00
15 6.99 7.73 0.36 0.13
30 6 48
6.48 7 16
7.16 0 78
0.78 0 28
0.28
60 5.54 6.12 1.53 0.55
120 4.73 5.23 2.18 0.79
240 4.03 4.46 2.75 0.99
500 3.40 3.76 3.25 1.17
9.00
FID signal is
8.00
7.00
6.00
5.00
EB/GB proportional to
mass concentration
BUT/GB
4.00
BB/GB
3.00
ETH/GB
2.00
1.00
0.00
0 100 200 300 400 500 600
AR
0 7.44 8.22 0.00 0.00
15 6.99 7.73 0.36 0.13
30 6 48
6.48 7 16
7.16 0 78
0.78 0 28
0.28
60 5.54 6.12 1.53 0.55
120 4.73 5.23 2.18 0.79
240 4.03 4.46 2.75 0.99
500 3.40 3.76 3.25 1.17
Calibration curve (FID)
Calibration curve (FID)
Weight Ratio
A
Area Ratio
R ti
ratio Area
Weight ratio α
Weight A ratio
ti
Weight ratio = (K) * Area ratio
Area (sec.volt) Concentration (mg/ml)
EB BUT BB ETH GB
Calibration 1 3 3 3 3 3
Calibration 1
Calibration 2
Calibration 3
EB BUT BB ETH GB
WR
Calibration 1 1 1 1 1
EB BUT BB ETH GB EB BUT BB ETH GB
Calibration 1 14398 24957 9359 10545 7487 3 3 3 3 3
Calibration 2 31758 55047 20643 23259 8257 6 6 6 6 3
Calibration 3 79933 138550 51956 58542 8313 15 15 15 15 3
WR
Calibration 1 14398 24957 9359 10545 7487 3 3 3 3 3
Calibration 2 31758 55047 20643 23259 8257 6 6 6 6 3
Calibration 3 79933 138550 51956 58542 8313 15 15 15 15 3
AR WR
EB/GB BUT/GB BB/GB ETH/GB
Calibration 1 1.92 3.33 1.25 1.41 1 1 1 1
Calibration 2 3.85 6.67 2.50 2.82 2 2 2 2
Calibration 3 9.62 16.67 6.25 7.04 5 5 5 5
C i
Calibration
i 1 14398 249
24957 93 9
9359 10 4
10545 7487
48 3 3 3 3 3
Calibration 2 31758 55047 20643 23259 8257 6 6 6 6 3
Calibration 3 79933 138550 51956 58542 8313 15 15 15 15 3
AR WR
Calibration 1 1 92
1.92 3 33
3.33 1 25
1.25 1 41
1.41 1 1 1 1
Calibration 2 3.85 6.67 2.50 2.82 2 2 2 2
Calibration 3 9.62 16.67 6.25 7.04 5 5 5 5
EB/GB
y = 0.52x
6 R² = 1
3 EB/GB
2 Linear (EB/GB)
0
0 2 4 6 8 10 12
EB BUT BBETH GB EB BUT BB ETH GB
Calibration 1 14398 24957 9359
10545 7487 3 3 3 3 3
Calibration 2 31758 55047 20643
23259 8257 6 6 6 6 3
Calibration 3 79933 138550 51956 58542 8313 15 15 15 15 3
AR WR
Calibration 1 1.92 3.33 1.25 1.41 1 1 1 1
Calibration 2 3.85 6.67 2.50 2.82 2 2 2 2
Calibration 3 9.62 16.67 6.25 7.04 5 5 5 5
WR/AR
0.52 0.30 0.80 0.71
AR
0 7.44 8.22 0.00 0.00
15 6.99 7.73 0.36 0.13
30 6.48 7.16 0.78 0.28
60 5.54 6.12 1.53 0.55
120 4.73 5.23 2.18 0.79
240 4.03 4.46 2.75 0.99
500 3.40 3.76 3.25 1.17
9.00
8.00
7.00
6.00
EB/GB
5.00
BUT/GB
4.00
BB/GB
3.00
ETH/GB
2.00
1.00
0.00
0 100 200 300 400 500 600
AR
0 7.44 8.22 0.00 0.00
15 6.99 7.73 0.36 0.13
30 6.48 7.16 0.78 0.28
60 5.54 6.12 1.53 0.55
120 4.73 5.23 2.18 0.79
240 4.03 4.46 2.75 0.99
500 3.40 3.76 3.25 1.17
WR/AR
0 52
0.52 0 30
0.30 0 80
0.80 0 71
0.71
AR
0 7.44 8.22 0.00 0.00
15 6.99 7.73 0.36 0.13
30 6.48 7.16 0.78 0.28
60 5.54 6.12 1.53 0.55
120 4.73 5.23 2.18 0.79
240 4.03 4.46 2.75 0.99
500 3.40 3.76 3.25 1.17
WR/AR
0 52
0.52 0 30
0.30 0 80
0.80 0 71
0.71
WR
0 3 87
3.87 2 47
2.47 0 00
0.00 0 00
0.00
15 3.63 2.32 0.29 0.09
30 3.37 2.15 0.62 0.20
60 2.88 1.84 1.23 0.39
120 2.46 1.57 1.75 0.56
240 2.10 1.34 2.20 0.70
500 1.77 1.13 2.60 0.83
WR
0 3 87
3.87 2 47
2.47 0 00
0.00 0 00
0.00
15 3.63 2.32 0.29 0.09
30 3.37 2.15 0.62 0.20
60 2.88 1.84 1.23 0.39
120 2.46 1.57 1.75 0.56
240 2.10 1.34 2.20 0.70
500 1.77 1.13 2.60 0.83
Weight of GB added 3 mg
WR
0 3 87
3.87 2 47
2.47 0 00
0.00 0 00
0.00
15 3.63 2.32 0.29 0.09
30 3.37 2.15 0.62 0.20
60 2.88 1.84 1.23 0.39
120 2.46 1.57 1.75 0.56
240 2.10 1.34 2.20 0.70
500 1.77 1.13 2.60 0.83
WT (mg)
0 11.60 7.40 0.00 0.00
15 10.90 6.95 0.87 0.28
30 10.10 6.44 1.86 0.59
60 8.64 5.51 3.68 1.18
120 7.38 4.71 5.24 1.67
240 6.29 4.01 6.59 2.11
500 5.31 3.39 7.81 2.49
Weight of GB added 3 mg
WR
0 3 87
3.87 2 47
2.47 0 00
0.00 0 00
0.00
15 3.63 2.32 0.29 0.09
30 3.37 2.15 0.62 0.20
60 2.88 1.84 1.23 0.39
120 2.46 1.57 1.75 0.56
240 2.10 1.34 2.20 0.70
500 1.77 1.13 2.60 0.83
WT (mg/ml)
0 11.60 7.40 0.00 0.00
15 10.90 6.95 0.87 0.28
30 10.10 6.44 1.86 0.59
60 8.64 5.51 3.68 1.18
120 7.38 4.71 5.24 1.67
240 6.29 4.01 6.59 2.11
500 5.31 3.39 7.81 2.49
WT (mg/ml)
0 11.60 7.40 0.00 0.00
15 10.90 6.95 0.87 0.28
30 10.10 6.44 1.86 0.59
60 8.64 5.51 3.68 1.18
120 7.38 4.71 5.24 1.67
240 6.29 4.01 6.59 2.11
500 5.31 3.39 7.81 2.49
116 74 144 46
WT (mg/ml)
0 11.60 7.40 0.00 0.00
15 10.90 6.95 0.87 0.28
30 10.10 6.44 1.86 0.59
60 8.64 5.51 3.68 1.18
120 7.38 4.71 5.24 1.67
240 6.29 4.01 6.59 2.11
500 5.31 3.39 7.81 2.49
116 74 144 46
mmol/ml = mol/liter =M
0 0.1000 0.1000 0.0000 0.0000
15 0.0940 0.0940 0.0060 0.0060
30 0.0871 0.0871 0.0129 0.0129
60 0.0745 0.0745 0.0255 0.0255
120 0 0636
0.0636 0 0636
0.0636 0 0364
0.0364 0 0364
0.0364
240 0.0542 0.0542 0.0458 0.0458
500 0.0458 0.0458 0.0542 0.0542
0.1200
0.1000
0.0800
EB
BUT
0.0600
BB
ETH
0.0400
0.0200
0.0000
0 0.1000 0.1000 0.0000 0.0000
15 0.0940 0.0940 0.0060 0.0060
30 0.0871 0.0871 0.0129 0.0129
60 0.0745 0.0745 0.0255 0.0255
120 0 0636
0.0636 0 0636
0.0636 0 0364
0.0364 0 0364
0.0364
240 0.0542 0.0542 0.0458 0.0458
500 0.0458 0.0458 0.0542 0.0542
Conversion
0 0.00 0.00 0.00 0.00
15 6.02 6.03 6.02 6.02
30 12.92 12.92 12.92 12.92
60 25.54 25.54 25.54 25.54
120 36 39
36.39 36 39
36.39 36 39
36.39 36 38
36.38
240 45.78 45.78 45.78 45.78
500 54.22 54.22 54.22 54.22
0 0.1000 0.1000 0.0000 0.0000
15 0.0940 0.0940 0.0060 0.0060
30 0.0871 0.0871 0.0129 0.0129
60 0.0745 0.0745 0.0255 0.0255
120 0 0636
0.0636 0 0636
0.0636 0 0364
0.0364 0 0364
0.0364
240 0.0542 0.0542 0.0458 0.0458
500 0.0458 0.0458 0.0542 0.0542
Conversion
0 0.00 0.00 0.00 0.00
15 6.02 6.03 6.02 6.02
30 12.92 12.92 12.92 12.92
60 25.54 25.54 25.54 25.54
120 36 39
36.39 36 39
36.39 36 39
36.39 36 38
36.38
240 45.78 45.78 45.78 45.78
500 54.22 54.22 54.22 54.22
60.00
50 00
50.00
40.00
EB
30.00 BUT
20.00 BB
ETH
10.00
0.00
0 100 200 300 400 500 600
‐10.00
Sample analysis (Split Injection)
Sample
Known weight of internal stander
Inject → Area Ratio
Calibration constant → Weight ratio
Sample weight
p g
conversion Sample concentration
Q. An Enzymatic transesterification of Ethyl Butyrate (EB) and
Butanol (BUT) to Butyl Butyrate (BB) and Ethanol (ETH) is carried
out in 15 liter reaction vessel with 10 liter of reaction mixture volume.
volume
1 ml of sample is taken out for analysis at different time intervals, 3
mg of Geraniol Butyrate (GB) is added as an internal stander to all
samples,
l andd then
h injected
i j d in
i GC which
hi h is
i mountedd withi h FID operatedd
with split ratio of 1:50. Following table gives area under picks for all
five compounds
p for different sample
p and three different calibratingg
samples. Observe the data carefully and fill the correct values for all
question marks in table. Write all the steps involved in calculation
showing all details.
details In both reaction and calibration hexane is used as
solvent . Draw the plot of time variation with time and find the value
of rate constant if reaction is assumed to be of 2nd order rate kinetics
Ethyl Butyrate (EB) + Butanol (BUT) Butyl Butyrate (BB) + ethanol (ETH)
Sampling Area under pick (sec.volt) Concentration (mg/ml)
Time (min) EB BUT BB ETH GB EB BUT BB ETH GB
0 48515 75785 0 0 6079 ? ? ? ? ?
15 39323 60994 1638 1846 5243 ? ? ? ? ?
30 52525 80982 4049 4562 7362 ? ? ? ? ?
60 49927 75058 11133 12544 8402 ? ? ? ? ?
120 33954 49714 12624 14224 6688 ? ? ? ? ?
240 23712 33611 13015 14665 5480 ? ? ? ? ?
500 27075 36803 20841 23482 7410 ? ? ? ? ?
Calibration 1 14398 24957 9359 10545 7487 3 3 3 3 3

Calibration 2 31758 55047 20643 23259 8257 6 6 6 6 3
Calibration 3 79933 138550 51956 58542 8313 15 15 15 15 3

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Case Study

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Fig: Schematic Representation of gas chromatography

Fig: Pictorial Representation of gas chromatography

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Ethyl Butyrate (EB) + Butanol (BUT)

Inject → Area Ratio

Calibration constant → Weight ratio

Calibration 1 14398 24957 9359 10545 7487 3 3 3 3 3

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