DISTILLATION EXPERIMENT - Monday 29th Feb 2016

Time
Comments

Sample Details
Density Bottle Wt
14:04 Start up rig. Cooling water on
Empty
14:06 Left side main reservior
S1
34.33
14:21 Righ side main reservior
S2
34.37
Bottom of reboiler after 7litres has been charged into
S3
34.33
DATA LOGGER STARTED
Samples taken from main nreserviors
14:22 Pump Left reservior into boiler
14:49 Reservior 1 transferred
14:49 Start transferring part of reservior 2 across
14:59 Transferr finsihed. Reboiler filled to 7 litres
15:00 Cooling water check - 100 litres/hr
15:02 Heating power to 100%, reflux to 100%
15:20 Bubbling on bottom tray. Reduced heating to 50%
15:22 Column DP now 1.1 mbar
15:23 No sign of liquid from reflux condenser
15:29 Column starting to stabilise. Liquid now from reflux condenser.
15:31 Temperatur and pressure profile from chart seemes that column is stable
15:33 T3, T4, T5 showing slight increases - not reached steady state
15:35 Reduce column heating to 35% - liquid level in condenser separator rising too quickly
15:40 Drop column heating to 25% - liuqid level in reflux collector still rising
15:44 Set column heater to 30% - temperature profile in plates above bottom plate are not varied
15:50 No - too high. Reduced heater power to 27%
16:03 Profiles suggest column is ok. Lot of bubbling on bottom tray. Ready to start 35% reflux
16:04 Set top 35% reflux
16:05 S4 Taken - from reflux collector, not from overhead cS4
34.33
16:15 S5 taken
S5
34.33
16:18 Moved the hose at the top of the column connecting to the Dp meter - looks like liquid is in
16:20 S6 taken
S6
34.36
16:25 S7 Taken
S7
34.34
16:27 Bubbling on bottom tray has stopped - more like small bubbles that you'd expect to see
16:30
S8
34.33
16:40
S9
34.28
16:45
S10
34.36
16:50
S11
34.33
16:55
S12
34.3
17:00
S13
34.31
17:05 1 Lire of reflux collected
S14
34.28
17:05 Total volume of liquid reflux collected has reached the 1 litre mark
17:17
S15
34.37
17:25
S16
17:43
S17
34.27
17:57
S18
34.34
18:00 Prepare for shut dow
18:03 Logging stopped

Batch at 35% Refllux, 27% Reboiler power

Spot Temperatures
Reflux collected
Main Reservior Contents at start of
ensity Bottle Wt
Reboiler
Top of Col L
(mm from base of Vessel V)
Left
Full (50ml)
T3
T12
Volume (L)
4.7
81.84
81.56
81.86

tor rising too quickly

bottom plate are not varied sufficient

ady to start 35% reflux

76.35
75.83
eter - looks like liquid is in the hose line
75.48
75.17
hat you'd expect to see
74.98
75.07
75.28
75.33
88.5
75.39
88.7
75.45
89
75.47
89.5
75.52
75.55
75.52
75.52

90.3
90.9
92.5
93.6

or Contents at start of charge

Right
5.1666667

DISTILLATION EXPERIMENT - Tuesday 1st March 2016

Time
Comments
9:13 Start up rig. Cooling water on
Left Reservior Sample
S1
9:26 Right Reservior Sample
S2
9:27 Start transfer pump - both reserviors open
9:33 Logging started
9:57 Transfer complete - reboiler holding 6L
9:58 Heating power set to 100%
10:14 Heavy bubbling on bottom plate
10:15 Bubbling on bottom plate reduced
10:16 Bubbling now steady
10:18 Condensate appearing in reflux collector
10:20 Reduced heating power to 50%
10:23 Reduce heating to 40% - reflux collector is almost full
10:35 teady state reached - bubbling small but stable. Collector looms stab
10:36 Reflux to 35%
10:40
S3
10:45
S4
10:50
S5
11:01
S6
11:07
S7
11:10
S8
11:20
S9
11:27
S10
11:30
S11
11:35
S12
11:40
S13
11:45
S14
11:50
S15
11:55 Level warning too low
S16
11:56 Shut Down - Set boiler to 0%, reflux to 100%
12:01 Drain down through cooler, empty reflux collector
12:01 Stop data logger

Sample Deta

Batch at 35% Refllux, 30% Reboiler power

Sample Details
Spot Temperatures
Reflux collected
Density Bottle Wt
Reboiler
Top of Col
L
(mm from base of Vessel V)
Empty
Full (50ml)
T3
T12
34.33
82.13
34.23
81.34

34.22
34.39
34.31
34.3
34.32
34.33
34.33
34.34
34.33
34.34
34.34
34.35
34.35

75.49
75.54
75.6
75.69
75.67
75.69
75.71
75.7
75.65
75.7
76.67
78.81
79.89
80.21

21.9
85.6

20.9
21

86.4

76.9

90.2
90.7
91.3
93
94.2
94.2
95.6
96.5
97
97.4
97.6
98.2
98.6
98.6

79.6
79.8
79.9
79.7
79.6
79.6
79.2
79.5
80.1
91.6
94.9
96
96.6
??

0.64
0.77
0.88
0.90
1.00
1.14
1.19
1.23
1.25
1.28
1.29
1.30

69
83
95
97
108
123
128
133
135
138
139
140

Main Reservior Contents at start of charge

Left
Right
Initial Vol
45
53 offsets from 4L mark
Base marks
58
56
Convert to volumes

DISTILLATION EXPERIMENT - Tuesday 1st March 2016

Time
Comments
12:14 Start up rig. Cooling water on
Left Reservior Sample

Sample Details
Density Bottle Wt
Empty
S1
34.31
S2
34.31

13:39 Start data logger

13:40 Start heating
13:56 Boiler temperature now 82.3 deg
13:57 Bubbling on the bottom plate
14:03 Set heater to 40%
14:05 Set heater to 45%
14:12 Looks like temperatures show steady state.
14:13 Switch reflux to 65%
14:15
S3
34.27
14:20
S4
34.34
14:30
S5
34.33
14:40
S6
34.32
14:50 More rigorus bubbling on bottom tray. Nothing on da S7
34.26
15:00
S8
34.32
15:10
S9
34.31
15:20
S10
34.31
15:29 Extract 0.5L from reflux vessel V and correct the depth for the volume removed
15:30 Correction applied to distilate volume using volume S11
34.35
15:48
S12
34.28
15:57
S13
34.31
16:00 Seeing refractive index change in overhead product indicating more water coming over
16:03 Graph shows standard 1st order control response
S14
34.32
16:06
S15
34.36
16:10
S16
34.33
16:12
S17
34.32
16:15 Shut down heater, 100% reflux on

Batch at 35% Refllux, 30% Reboiler power

Spot Temperatures
Reflux collected
Main Reservior Contents at star
ensity Bottle Wt
Reboiler
Top of Col L
(mm from base of Vessel V)
Full (50ml) T3
T12
Volume
81.56
81.41

84.7

25.3

86.1

78.8

79.94
87.2
77.37
87.5
76.12
88.8
75.81
90.3
75.73
92.1
75.63
93.6
75.58
94.8
75.62
96.8
e volume removed
75.58
97.7
75.52
99
75.72
99.2
g more water coming over
78.01
99.6
78.85
99.9
80.52
99.8
81.27
100

79.5
79.6
79.7
79.7
79.7
79.5
79.4
79.4

0.35
0.41
0.66
0.90
1.08
1.20
1.32
1.50

28
35
62
87
107
120
133
152

79.2
79.5
97.2

1.57
1.72
1.84

8
24
37

97.9
98.4
98.7
98.5

1.88
1.88
1.88
1.88

41
41
41
41

ain Reservior Contents at start of charge

Left
Right
5
5 Litres

DISTILLATION EXPERIMENT - Thursday 3rd March 2016

Time
Comments
Sample Details
Density Bottle Wt
13:59 Start up rig. Cooling water on
Empty
S1
34.3
S2
34.3
14:15 Start transfer pump to reboiler
14:27 Data logging started
14:41 Transfer pump stopped. Reboiler holding 5.5L
14:42 Reflux set to100%, heating turned on to 100%
14:51
15:00 Bubbling on the 1st plate - this disapears quickly
15:03 Turn heater power to 45%
15:12 Pump feed to 50%, refluxc to 35%
15:13
S3 (Cond)
15:16
S4 (Reb)
15:17
S5 (Cond)
15:22
S6 (Cond)
15:23 Low level swicth off
Heating restarted
S7(Reb)
15:33
S8(Cond)
15:37
S9(Reb)
15:40
S10(Reb)
S11(Cond)
Reflux collector vessel fiull - drained off to 1.5L
15:45 Increased cooling water flowrate to condenser
Level shut down on heater
15:46 Shut down rig

Continious at 35% Refllux, 45% Reboiler power

Spot Temperatures
Reflux collected
Main Reservior Contents at star
ensity Bottle Wt
Reboiler
Top of Col L
(mm from base of Vess
Full (50ml) T3
T12
Volume
81.44
Base marks
82.04
Level of Liquid in Main Reservio
Depth (mm)
Left
148

82
82.36
80.06
79.03
82.25
79.33
82.39
82.4
79.45

88.5
89.3
89.3

81.2
82
82.01

85.5
87.8
88.8
89.5

0.19

11

116

74.4
81.7
82.5

0.86
1.46

83
148

70
68

82.4

1.51

153

62

ain Reservior Contents at start of charge

Left
Right
5
5 Litres
ase marks

evel of Liquid in Main Reservior Tanks During Run

Depth (mm)
Right

Volume (L)
Left
Right
120

106

73
50
35