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    DISTILLATION EXPERIMENT - Monday 29th Feb 2016

    Uploaded by

    Ahmad
    The document describes a distillation experiment conducted over multiple days. On the first day, samples were taken from the distillation column every 15-30 minutes as temperatures and flow rates were adjusted to achieve steady state operation at 35% reflux and 27% heating. The second day involved a similar process to reach steady state at 35% reflux and 30% heating. On the third day, samples were taken every 10-20 minutes as the column was operated at 65% reflux and various heating levels to reach steady state.

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    © All Rights Reserved
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    DISTILLATION EXPERIMENT - Monday 29th Feb 2016

    Uploaded by

    Ahmad
    23 views12 pages
    The document describes a distillation experiment conducted over multiple days. On the first day, samples were taken from the distillation column every 15-30 minutes as temperatures and flow rates were adjusted to achieve steady state operation at 35% reflux and 27% heating. The second day involved a similar process to reach steady state at 35% reflux and 30% heating. On the third day, samples were taken every 10-20 minutes as the column was operated at 65% reflux and various heating levels to reach steady state.

    Original Description:

    hj

    Original Title

    Set 1

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    The document describes a distillation experiment conducted over multiple days. On the first day, samples were taken from the distillation column every 15-30 minutes as temperatures and flow rates were adjusted to achieve steady state operation at 35% reflux and 27% heating. The second day involved a similar process to reach steady state at 35% reflux and 30% heating. On the third day, samples were taken every 10-20 minutes as the column was operated at 65% reflux and various heating levels to reach steady state.

    Copyright:

    © All Rights Reserved
    Download as XLSX, PDF, TXT or read online from Scribd
    Download as xlsx, pdf, or txt
    23 views12 pages

    DISTILLATION EXPERIMENT - Monday 29th Feb 2016

    Uploaded by

    Ahmad
    The document describes a distillation experiment conducted over multiple days. On the first day, samples were taken from the distillation column every 15-30 minutes as temperatures and flow rates were adjusted to achieve steady state operation at 35% reflux and 27% heating. The second day involved a similar process to reach steady state at 35% reflux and 30% heating. On the third day, samples were taken every 10-20 minutes as the column was operated at 65% reflux and various heating levels to reach steady state.

    Copyright:

    © All Rights Reserved
    Download as XLSX, PDF, TXT or read online from Scribd
    Download as xlsx, pdf, or txt
    of 12

    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

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