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A. Preparation and checking procedures (a few days before experiment).... 8
   1. Check the installation. ........................................................................................................ 8
      a) Check whether all pipes and vessels are clean. .............................................................. 8
      b) Check whether all valves are clean and functional. ....................................................... 8
      c) Check whether all parts are installed properly. .............................................................. 8
      d) Do the "pressure-test". ................................................................................................... 8
   2. Check the heatings. ............................................................................................................ 8
      a) Switch on the temperature console. ............................................................................... 8
      b) Test the heating of the effluent line and the sampling pipes for the C4- analysis. ......... 8
      c) Test the heating of the sampling pipes for the C5+ analysis. .......................................... 9
      d) Test the heating of the C5+ oven.................................................................................... 9
      e) Test the heating of the pressure regulation valve. .......................................................... 9
      f) Test the heating of the heavy HC feeding system. ......................................................... 9
   3. Analysis part preparation ................................................................................................... 9
      a) Check amount of analytical gases. ................................................................................. 9
      b) Order liquid nitrogen needed for C5+ analysis. .............................................................. 9
      c) Check amount of calibration gases (HC calibration mixtures). ................................... 10
      d) Check amount of the nitrogen used as internal standard. ............................................ 10
      e) Check function of GCs for the C5+ analysis. ................................................................ 10
      f) Do calibration of GCs for the C4- analysis. .................................................................. 10
   4. Check the sampling system. ............................................................................................. 10
      a) Test whether C4- sample loops are free. ....................................................................... 10
      b) Check cleanness and permeability of C5+ sample loops .............................................. 11
   5. Find setting parameters. ................................................................................................... 11
B. Check vessels and valve setting before experiment. .................................. 11
   1. Set and check valves position........................................................................................... 11
      a) Check whether the valve K150 is fully open. If not open it. ....................................... 11
      b) Check whether the valve K151 is closed. If not, close it. ............................................ 11
      c) Prepare the IR sampling system for carbon oxides analysis. ....................................... 12
      d) Check whether valves K142, K138, K137 and 139 are open. If not open them. ......... 12
      e) Check whether valves K131 and K134 are closed. If not close them. ......................... 12

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August 2005                                                                                                              Michael Lottin
      f) Check whether valves K132 and K133 are closed. If not close them. ......................... 12
      g) Check whether the valve K105 is open. If not open it. ................................................ 12
      h) Close the valve K130. .................................................................................................. 12
      i) Prepare the C4- injection system. .................................................................................. 12
      j) Prepare the C5+ injection system. .................................................................................. 12
      k) Connect or disconnect TLE1. ...................................................................................... 13
   2. Fill up all operational vessels, which you are going to use. ............................................. 13
      a) Apply overpressure to storage barrels (max. 0.2bar). .................................................. 13
      b) Feed the water operational storage vessel. ................................................................... 13
      c) Feed the naphtha operational storage vessel. ............................................................... 13
      d) Feed the operational storage vessel for heavy HC. ...................................................... 13
      e) Feed the operational storage vessel for liquefied HC gases. ........................................ 14
      f) Check the battery for feeding HC gases ....................................................................... 14
      g) Check the bottles with gas used to decoke................................................................... 14
      h) Check the storage amount of all another liquids and gases necessary for experiment. 14
C. Heating-up of the furnace ............................................................................ 15
   1. Start-Up the reactor .......................................................................................................... 15
      a) Preparation. .................................................................................................................. 15
      b) Heating up (three persons are required). ...................................................................... 15
      c) Resetting of SIEGER alarm cupboard ......................................................................... 16
   2. Operation during the day or night .................................................................................... 16
      a) Operation during the day .............................................................................................. 16
      b) Operation during the night ........................................................................................... 17
D. Cooling down and shut down of the reactor .............................................. 17
E. Feeding ........................................................................................................... 18
   1. Feeding system preparation. ............................................................................................. 18
      a) Water feeding. .............................................................................................................. 18
      b) Feeding of the internal standard (N2) at the reactor output. ......................................... 18
      c) Combustion controller .................................................................................................. 18
      d) heat-up the “butane” line (if necessary). ...................................................................... 19
      e) heat-up the heavy HC feeding section (if necessary). .................................................. 19
      f) apply pressure in all storage vessels which are going to be used ................................. 19
      g) Prepare vessels for naphtha, water and heavy HC. ...................................................... 19

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August 2005                                                                                                                 Michael Lottin
      h) Check amount of nitrogen used as the overpressure gas for feeding of liquids. ......... 19
   2. Hydrocarbon feeding systems .......................................................................................... 20
      a) Feeding of liquefied gasses .......................................................................................... 20
      b) Feeding of liquid hydrocarbons ................................................................................... 20
      c) Feeding of heavy hydrocarbons ................................................................................... 20
      d) Feeding of gasses (butane) ........................................................................................... 20
   3. Preparation of outlet section for a feeding ....................................................................... 20
      a) “Turn ON” the TLE1 (if is necessary) ......................................................................... 20
      b) Switch on the heatings of the exit pipe and sampling systems. ................................... 21
      c) “Turn ON” the TLE2 and water condenser.................................................................. 21
      d) “Turn ON” the heating of PRV .................................................................................... 21
      e) Check the valve setting ................................................................................................ 21
      f) Switch on the water cooler for C4- effluent. ................................................................. 21
      g) Refill the water absorbers. ........................................................................................... 21
      h) Switch on the Lauda cooler.......................................................................................... 21
      i) Switch "ON" TCD bridges on "Agilent GC" and "Fisons GC". ................................... 22
      j) Check flame from FI detectors on "Agilent GC" and GCs for C5+ analysis. .............. 22
      k) Check whether "GC servers" are switched "ON". ....................................................... 22
      l) Start data acquisition. .................................................................................................... 22
F. Start cracking experiment............................................................................ 22
   1. Ignition of the flare ........................................................................................................... 22
   2. Preparation for cracking experiment ................................................................................ 23
   3. Start cracking experiment................................................................................................. 23
   4. Run analysis. (Do injection.) ............................................................................................ 24
      a) Start C4- analyses. ......................................................................................................... 24
      b) Start C5+ analyses. ........................................................................................................ 24
      c) Display chromatograms. .............................................................................................. 24
   5. Stop cracking experiment ................................................................................................. 24
G. Decoking ........................................................................................................ 25
   1. Preparation for decoking .................................................................................................. 25
   2. Start decoking experiment ................................................................................................ 26
   3. Stop the decoking experiment .......................................................................................... 26
   4. Collection of cokes on the filter ....................................................................................... 26

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August 2005                                                                                                                Michael Lottin
H. Sampling system for carbon oxides analysis with IR-analyser. .............. 27
      a) Valve settings during cracking. .................................................................................... 27
      b) Valve settings during decoking. ................................................................................... 27
I. Calibration procedures ................................................................................. 28
   1. How to calibrate C4 --GC’s .............................................................................................. 28
      a) Purge sample loops with calibration gas. ..................................................................... 28
      b) Check whether calibration gas is flowing through sample loops. ............................... 28
      c) Inject calibration gas. ................................................................................................... 28
      d) Wait 4 min and check status of all channels. ............................................................... 28
   2. How to calibrate COx analyser (once per day) ................................................................ 28
      a) Feed nitrogen. ............................................................................................................... 28
      b) Do zero calibration. ...................................................................................................... 29
      c) Do span calibration. ..................................................................................................... 29
J. Pressure test ................................................................................................... 30
      a) Valve setting................................................................................................................. 30
      b) Set reactor under pressure (up to 3 bar) with N2 .......................................................... 30
      c) Pressure has to be stable for at least 1 hour ................................................................. 30
K. X-Chrom user guide ..................................................................................... 30
   1. How to prepare X-Chrom ................................................................................................. 30
      a) Start up X-Chrom software. ......................................................................................... 30
      b) Start up X-Chrom software. ......................................................................................... 30
      c) Prepare all channels for injection. ................................................................................ 30
      d) Check whether "GC servers" are switched "on". ......................................................... 31
   2. How to work with X-Chrom ............................................................................................ 31
      a) Display chromatograms. .............................................................................................. 31
      b) Calculate peak areas for C4- components. .................................................................... 31
      c) Don't forget to set methane yields in the "Analysis method" for C5+ components. ..... 32
      d) Calculate peak areas for C5+ components. ................................................................... 32
L. LabView user guide ...................................................................................... 32
      a) Start up LabView software........................................................................................... 32
      b) Flowsheet window ....................................................................................................... 32
      c) Profile window ............................................................................................................. 33


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      d) Environment window ................................................................................................... 33
      e) CO-CO2 window .......................................................................................................... 33
      f) Burner press window .................................................................................................... 33
      g) Service window ............................................................................................................ 33
      h) Time based scheduling ................................................................................................. 33
M. Evaluation of results .................................................................................... 34
   1. How to calculate calibration factors for C4--GC’s .......................................................... 34
      a) Start EXCEL and open the calib file (with macro enabled)......................................... 34
      b) In sheet “bottle I, C1-C2”. ............................................................................................. 34
      c) In sheet “bottle II, C1-C4”............................................................................................. 34
      d) In sheet “Comparison”. ................................................................................................ 34
   2. How to make report of results C4--analysis ..................................................................... 34
      a) Start EXCEL and open the template file (with macro enabled). .................................. 34
      b) Save file as C4min-yyyymmdd.xls .............................................................................. 34
      c) In sheet “Status”. .......................................................................................................... 35
      d) In sheet “CF”................................................................................................................ 35
      e) In sheet “Peak Areas”................................................................................................... 35
      g) In sheet “Air” ............................................................................................................... 35
   3. How to make report of results C5+-analysis .................................................................... 35
      a) Start EXCEL and open the template file (with macro enabled). .................................. 35
      b) Save file as C5plus-yyyymmdd.xls.............................................................................. 35
      c) In sheet “Calcult”. ........................................................................................................ 36
      d) In sheet “Report”.......................................................................................................... 36
      e) In sheet “Calcult”. ........................................................................................................ 36
      f) In sheet “List”. .............................................................................................................. 36
   4. How to write final report .................................................................................................. 36
      a) Start EXCEL and open the template file. ..................................................................... 36
      b) Save file as results-yyyymmdd. After saving you can make changes. ........................ 36
      c) Clear all old data by pressing button "Clear all old data" in sheet “source Data”. ...... 36
      d) In sheet “Condition 1” ................................................................................................. 37
      e) In sheet “Source Data”. ................................................................................................ 37
      f) In sheet “Condition 1”. ................................................................................................. 37
      g) In sheet “Source Data”. ................................................................................................ 37


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August 2005                                                                                                                 Michael Lottin
   5. How to make cracking report for CO-CO2 ...................................................................... 38
   6. How to make decoking report for CO-CO2 ..................................................................... 38
N. Basics of GC’s ............................................................................................... 39
   1. Specifications for C5+-GC’s ............................................................................................ 39
      a) Type Hewlett Packard 5980 Series II. .......................................................................... 39
      b) Specifications for inlet flows ....................................................................................... 39
      c) Specifications for cooling system ................................................................................ 39
      d) Starting and stopping analyses ..................................................................................... 40
      e) Temperature program ................................................................................................... 40
   2. HP Agilent 6890N GC for C4—section ............................................................................. 41
      a) General information ..................................................................................................... 41
      b) Ignition FID ................................................................................................................. 41
      c) Starting analyses........................................................................................................... 41
      d) Reactivation of the columns......................................................................................... 41
   3. Interscience Fisons GC 8340............................................................................................ 42
      a) General information ..................................................................................................... 42
      b) Before analyses. ........................................................................................................... 42
      c) Starting analyses........................................................................................................... 43
O. Gas control panel.......................................................................................... 43
      a) Applications for nitrogen ............................................................................................. 43
      b) Applications for helium ............................................................................................... 43
      c) Applications for hydrogen............................................................................................ 43
      d) Applications for air ...................................................................................................... 44
P. Alarm conditions ........................................................................................... 44
      a) Failing of the exhaust gases venting ............................................................................ 44
      b) Flame deflection........................................................................................................... 44
      c) Back-fire ....................................................................................................................... 45
      d) High and low natural gas pressure ............................................................................... 45
      e) Over heating reactor ..................................................................................................... 45
      f) High pressure at inlet reactor ........................................................................................ 45
Q. Appendix 1 .................................................................................................... 46
R. Appendix 2 .................................................................................................... 47


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August 2005                                                                                                                   Michael Lottin
S. Appendix 3 ..................................................................................................... 48
T. Appendix 4 ..................................................................................................... 49
U. Appendix 5 .................................................................................................... 50
V. Appendix 6 .................................................................................................... 51




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August 2005                                                                                              Michael Lottin
A. Preparation and checking procedures (a few days before
experiment)
Procedure object: prepare all devices for experiment and check whether working properly.

1. Check the installation.
Whenever any parts were removed and cleaned or disconnected check closeness of
connections.
a) Check whether all pipes and vessels are clean.
b) Check whether all valves are clean and functional.
c) Check whether all parts are installed properly.
d) Do the "pressure-test".
For detailed information see chapter J



2. Check the heatings.
If you are going to switch on any heating wires, for the first time after cleaning, make sure
that all wires are connected correctly. Check connections and isolation of heating wires if
they’re not damaged.


a) Switch on the temperature console.
The console is situated on the left side of upper GC for the C5+ analysis. By this console you
can check temperatures at some points where are placed thermocouples connected with this
unit. Just press button with your number (see legend on the console).


b) Test the heating of the effluent line and the sampling pipes for the C4- analysis.
Heating of the pipe is important as a prevention of the condensation of liquids inside. If
everything is connected and isolated, run pipes heating. At first turn regulators to zero
(regulators “Habia cycloonleiding” and “Habia effluentleiding” are situated in the heating
control panel. Switch heating on. After that green light is lighting. Set the electric current
maximally at 2.5A. If you are turning with regulators and amperes are still on zero, wire is
probably disconnected. In this case immediately switch heating off.




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August 2005                                                                             Michael Lottin
c) Test the heating of the sampling pipes for the C5+ analysis.
The voltage regulator for heating of the C5+ sampling pipes is situated near the wall behind
C5+ chromatographs. At first turn voltage regulator at zero. Then put power switch to position
1 and set appropriate voltage on transformer (at marked position). After positive test keep
heating of the C5+ sampling system on.
The temperatures of the sampling line can be checked on the Pilot control panel


d) Test the heating of the C5+ oven.
The heating of the C5+ oven is regulated by two temperature controllers situated below the
oven. Put the controllers “ON” by means of the main switch and set temperature to 275 °C.


e) Test the heating of the pressure regulation valve.
The heating of the pressure regulation valve is regulated by the ‘temperature controller’
situated on the heating control panel. After positive test keep heating of the pressure
regulation valve on. Set point here is 150 °C.


f) Test the heating of the heavy HC feeding system.
Control panel for heating of heavy HC feeding system is located behind the pilot. At first turn
voltage regulators at zero position. Then put all necessary power switches to position 1 (green
light is lighting) and set appropriate voltage on transformers (at marked position). After
positive test keep on heating of all lines and balance vessel with the heavy HC.



3. Analysis part preparation
a) Check amount of analytical gases.
The pressurised bottles with analytical gases hydrogen and helium are situated behind the gas
control panel, only AIR is used from the air distribution net and nitrogen is taken from a
battery outside. Check amounts of gases in bottles on manometers and change bottle if it is
necessary.
For further information about the gas control panel refer to chapter O


b) Order liquid nitrogen needed for C5+ analysis.
Ask Michael to order liquid nitrogen. A full ranger is approximately 3.5 vessels.


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August 2005                                                                          Michael Lottin
c) Check amount of calibration gases (HC calibration mixtures).
Check pressure in the two calibration bottles with the calibration gas for TC detectors
calibration (bottle in standing position). Check weight difference of the calibration bottle
(bottle in horizontal position), which is used for the calibration of the FID channel. This
calibration mixture is in liquid stay and output pressure doesn't depend on liquid amount in
bottle.


d) Check amount of the nitrogen used as internal standard.
Internal standard is taken from the battery outside. Check pressure on the gas control panel.


e) Check function of GCs for the C5+ analysis.
Inject the mixture from the bottle with the calibration mixture for the FID calibration.


f) Do calibration of GCs for the C4- analysis.
How to do calibration refer to chapter I.1.



4. Check the sampling system.
Suggestion: For this tests use He. The calibration mixture is more expensive.


a) Test whether C4- sample loops are free.
Check whether the C4- sampling system is heated-up. If not, switch heating on.
For more information refer to chapter Error! Reference source not found.Fout!
Verwijzingsbron niet gevonden.
Connect a bottle with pressurised He and close valves K164, K167, K168. Switch the valve
under K167 to the right. Open valve K160.
Turn valves K161 and K162 at position "down" - feeding of sample loops from the N2 bottle.
Open the bottle. Check the pressure in the connected bottle and set output pressure
(0.5bar<P<0.8bar). Set the overpressure in the sampling system at 0.5bar by the valve K167.
Check the pressure on P160. Note: higher pressure is dangerous - glass parts are installed.
Check bubbles in the gas washing bottles for Fisons and HP Agilent GC. If you see bubbles
close the bottle. After when the pressure falls down close all valves, which have been opened.




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August 2005                                                                            Michael Lottin
b) Check cleanness and permeability of C5+ sample loops
Check if the C5+ injection system is heated-up. If not, switch it on.
For more information refer to chapter A.2. c)
Connect a bottle with pressurised He and close valves K167 and K168. Switch the valve
under K168 to the right. Open the bottle and set output pressure (0.8bar<P<1bar). Set
overpressure at 0.7 bar by valve K168. Check the pressure on P161.
For testing of the sample loop connected to valve K122 open valve K110. K122 has to be
‘OFF’, in purging position. Check bubbles in the gas washing bottle above the C 5+ oven.
Close the He bottle and when the pressure has fallen down close all valves which have been
opened.
Repeat the same actions to check the sample loop connected to valve K123. Therefore open
valve K111.



5. Find setting parameters.
Operational parameters as temperature profile, pressures, rate of flows as internal standard,
feed …



B. Check vessels and valve setting before experiment.

1. Set and check valves position.
Procedure object: open the way from the pilot output to the flare and close other outputs.


a) Check whether the valve K150 is fully open. If not open it.
At the beginning of the experiment this valve has to be open. This throttle valve is used to set
the pressure in the sampling part of the output pipe. To check this pressure open valve K140
to manometer P140.


b) Check whether the valve K151 is closed. If not, close it.
The valve K151 is opened only during the sampling as a prevention of impurities (cracking
residues) deposition. (After sampling purge sampling pipe by He.)



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August 2005                                                                          Michael Lottin
c) Prepare the IR sampling system for carbon oxides analysis.
For further information refer to chapter H


d) Check whether valves K142, K138, K137 and 139 are open. If not open them.
Open bypass of the pressure regulation valve. At the beginning of the experiment bypass has
to be open for in case that the pressure regulation valve doesn't work properly.


e) Check whether valves K131 and K134 are closed. If not close them.
The function of the valve K131 is venting of the accumulation vessel. By valve K134 the
accumulation vessel is connected to an air source to apply an overpressure in order to remove
the liquids accumulated in the vessel.
.
f) Check whether valves K132 and K133 are closed. If not close them.
The function of valves K132, K133 is to drain condensed liquids form separator and the water
cooler. Check these vessels whether they are empty.


g) Check whether the valve K105 is open. If not open it.
Important for the pressure control above TLE2 on manometer P101.


h) Close the valve K130.
The valve K130 is a vent valve.


i) Prepare the C4- injection system.
Turn valves K161 and K162 at position "up" - feeding of sample loops from the effluent line.
Check whether valve K160 to manometer P160 is open and K164 is closed.
Check whether valves K153 and K154 are closed.
Close also valve K151. This valve has to be opened only before purging and injection with
effluent which is regulated automatically by means of M150. Also the He purge is regulated
automatically by M151.


j) Prepare the C5+ injection system.




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August 2005                                                                        Michael Lottin
Check whether valves K110, K111 are closed. If not, close them. K120, K121 have to be
OFF, position closed. Valves K120 and K121 are only ON, position open to purge with
effluent. Valves K110 and K111 are only open to purge with He after sampling to prevent
deposition of impurities (cracking residues).


k) Connect or disconnect TLE1.
This is an air cooled transfer line exchanger.




2. Fill up all operational vessels, which you are going to use.


a) Apply overpressure to storage barrels (max. 0.2bar).
For feeding of some operational vessels it is necessary to apply overpressure to the main
storage barrels which you are going to use. To apply this pressure refer to chapter O.
Check whether K24 is open and the overpressure is max. 0.2 bar
If you applied higher pressure storage barrels could be damaged.


b) Feed the water operational storage vessel.
Open K14 (K15) to apply pressure in the 200 litre water barrel
If one of these 200 litre barrels is empty switch to the second one and warn Andre or Michael
Open K16 (K17) to let water flow to “weighted” vessel
Fill up the vessel by pressing the yellow button above the level checker (open M10) or switch
on the “Auto fill” function.


c) Feed the naphtha operational storage vessel.
Open K23 to apply pressure in the 200/25 litre naphtha barrel
Open K20 to apply pressure in naphtha weighted vessel
By pressing the yellow button above the level checker (open M22 and M21 and closes M20)
fill up the vessel. Check the level.


d) Feed the operational storage vessel for heavy HC.




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August 2005                                                                          Michael Lottin
Switch on the heating of pipes and vessels. For more information refer to chapter A.2. f) .
Wait until the sample is warmed up enough.
Open K42 to apply pressure in heavy HC barrel
Close the vent of the barrel
Close the venting valve, open the unmarked valve (the overpressure "source") and the valve
K34. By pressing the yellow button (open M30 and M31) fill up the vessel. Check the level of
the liquid in the vessel.


e) Feed the operational storage vessel for liquefied HC gases.
Open the valve K7. Location of the valve is second pillar. Bottles are outside. Gases are still
under pressure. By pressing the yellow button (open M1 and M4) fill up the vessel. (mass
balances missing, level checker missing).


f) Check the battery for feeding HC gases
This battery is situated behind the pilot
It can be used to feed propane, propene, butane and ethane
All these gases are fed through a MFC
Connect four bottles of the proper gas you want to use
Outlet pressure has to be approx. 5 bar
Open the valves K66 and K64 to start feeding to the reactor


g) Check the bottles with gas used to decoke
Air and Nitrogen are the proper gases
Outlet pressure has to be approx. 5 bar
The bottles are situated behind the pilot
Open the valves K66 and K64 to start feeding to the reactor


h) Check the storage amount of all another liquids and gases necessary for experiment.
Pressurised HC - check pressure in bottles.
Gases necessary for analysis. (H2, He, N2)




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August 2005                                                                          Michael Lottin
C. Heating-up of the furnace

1. Start-Up the reactor


a) Preparation.
Close all burner valves with exception of nr. 12 (cell 7)
Set all automatic control valves of the natural gas at their minimum position
Apply pressure in the 200 l water vessel with N2
Close the manual stop-cock (= big yellow handle)
Open the valves K132 and K133 (under TLE2)
Open the stand-by valve (above TLE2)
Open the valve K139 (above the cyclone)
Put the heating (HABIA) of the exit pipe on (situated on the heating control panel, set all
values to 2.5 A)


b) Heating up (three persons are required).
Main switch on AAN
Alarm on UIT and switch on DAG
Switch on MANUEEL (autofiring is OFF)
Put on the computer to record the temperatures in the furnace and start the water pump
Put the balance on
Control the water level and if necessary, fill by means of the yellow button (above the
balance) or switch on the “Auto fill” option
Open K10 to start pumping water through the reactor
Open the main natural gas-supply
Start the combustion controller (= compressor outside). At this moment also the vacuum
pump upstairs will start (gas pressure has to be approxiamately 0.2 kp/cm²)
The oil pump (for cooling TLE2) has to be started once you’re feeding
Open slowly the manual stop-cock (= big yellow handle)
“Mix valve” lights up on the main control panel
Open the Maxon valve, which is used for the natural gas supply
“Maxon kraan” lights up on the main control panel




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August 2005                                                                        Michael Lottin
Put burner press manually to 30 in cell 7 to ignite burner 12. The burner has to be on within 2
minutes after opening the Maxon valve. If this is not the case, close the maxon valve, purge
with air during 15 minutes and try again.
Open one by one the burner valves and ignite burner 11-10-9-8-7 (cell 7)
The same for cells 6-5-4-3-2
For cell 1 ignite only burners 13-15-18
Open one by one the burner valves and ignite burners 1-2-3-4-5-6 (cell 7)
Repeat the same action for cells 6-5-4-3-2
For cell 1 ignite only burners 2-4-7-9


If too much methane is detected during ignition of the burners, reset the SIEGER alarm
cupboard


c) Resetting of SIEGER alarm cupboard
Press the RESET button on the control panel
If all alarm conditions are disappeared, switch the alarm on AAN and audio on AAN
Heat the furnace by means of the automatic control valves of the natural gas (manually or by
setting the temperature profile on the computer)

2. Operation during the day or night


a) Operation during the day
Close the stand-by valve above TLE2 and open valve K139 (safety valve which prevents
condense can get into the effluent line during night)
Drain off the superfluous condense water with valves K132 and K133 after every run
Switch DAG, Autofiring, Audio and Alarm ON
Switch on the oil pump for cooling TLE2
In an alarm situation, only the alarm is mentioned and 15 minutes later the combustion
controller is switched off
So, within 15 minutes, a manual intervention has to stop the alarm situation




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August 2005                                                                          Michael Lottin
b) Operation during the night
Open the stand-by valve above TLE2, close valve K139 (safety valve which prevents
condense can get into the effluent line during night) and open valves K132 and K133 to drain
off the superfluous condense water during the night
Switch DAG OFF
Switch Autofiring OFF and set all gas pressures manually to 10
This can also be done with Autofiring ON but then the computer can reset the pressures
Switch Audio OFF
Put water feed to zero
Switch off the oil pump for cooling TLE2
Only Alarm has to stay ON
In an alarm situation, the MAXON valve immediately switches off, so that the furnace is
immediately shut down and 15 minutes later, the combustion controller, the vacuum pump
and the oil pump are switched off




D. Cooling down and shut down of the reactor


Set temperature profile on PC so that the automatic control valves of the natural gas go to
their minimum (temp. will decrease with approximately 6 °C/min)
Switch the button on the control panel on the position DAG
Close the valve of the gas supply
The Maxon valve immediately switches off and 15 minutes later, the combustion controller,
the vacuum pump and the oil pump are switched off
Switch off the main switch on the control panel
Release pressure on the 200 liter water vessel
Switch off the outlet pressure regulation
Switch off the heating (Habia wiring) of the outlet pipe




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August 2005                                                                       Michael Lottin
     Emergency shut-down


     In case of an emergency set the main switch HOOFDSCHAKELAAR on UIT
     (see control panel)




E. Feeding
water always the first to start and the last to stop!

1. Feeding system preparation.
a) Water feeding.
Check if the Autofill function is ON
The balance vessel can also be filled manually with the yellow button Fill (above the balance)
Check if the pressure is applied in the 200 liter water barrel, for details refer to chapter B.2.
Set water flow manually on Hitachi J100 panel (display in Hz) or automatically by computer
(display in g/hour) → 1008 g/h is 7.0 Hz, 1155 g/h is 7.8 Hz, 4000 g/h is 26.5 Hz
Open the valve K13
The mity mite is used to control the pulsations of the pump. Pressure on P11 has to be around
7 bar. Therefore open the gassupply on the gac control panel. Also K11 has to be open, K12
closed (only used to lose the pressure)


b) Feeding of the internal standard (N2) at the reactor output.
Set 70% (usually) on the channel 1 on the bottom mass flow controller (Brooks) and open the
valve K100. Nitrogen is fed from the battery outside (check output pressure, 5bar is
maximal). Use selector on the mass flow controller (Brooks) to display the actual value and if
it's necessary correct it to 70%.


c) Combustion controller
The combustion controller is used to feed the burners with the gas air mixture.


Manual Pilot                                                                                        18
August 2005                                                                              Michael Lottin
This mixture can be regulated outside with the appropriate button
By means of a timer the combustion controller is greased with oil
Every 8 hours (at 8, 17 and 1 o’clock) the timer, which is situated in the electrical closet
behind C5+ GC’s, gives a pulse of 5 seconds through output 1 which results in adding a few
drops of oil from the reservoir to the combustion controller
Always keep an eye on the oil level


d) heat-up the “butane” line (if necessary).
Turn on HAB4 + HAB5 to heat up tube from MFC to reactor


e) heat-up the heavy HC feeding section (if necessary).
Install heating and insulation on the barrel
Let vent the barrel during heating-up
Heat-up the weighted vessel
Turn ON the control unit on the heating control panel
Set temperature ???°C
Heat-up the pump
Turn ON the oil bath nearby
Set temperature ???°C
Turn ON the HABIA heating
Turn on HAB3 to heat-up tube from the barrel to the pump
Turn on HAB1 +HAB2 to heat-up the line from the pump to the reactor


f) apply pressure in all storage vessels which are going to be used
For more information refer to chapter B.2.


g) Prepare vessels for naphtha, water and heavy HC.
If you want to use "new" liquid hydrocarbon feeds (naphtha, heavy HC), then clean-up
operational storage vessels.


h) Check amount of nitrogen used as the overpressure gas for feeding of liquids.
Main manometer for nitrogen on Gas Control Panel has to be on approximately 13 bar




Manual Pilot                                                                                  19
August 2005                                                                        Michael Lottin
2. Hydrocarbon feeding systems


a) Feeding of liquefied gasses
The battery for feeding of liquefied gasses is situated at the backside of the Pilot.
The feeding is controlled by means of specified MFC’s for the different gasses.


b) Feeding of liquid hydrocarbons
The balance vessel for liquid hydrocarbons is situated next to the water balance vessel.
From here the hydrocarbons are pumped into the reactor
A Danfoss controller is used to control the pump.
Set flow manually (display in Hz) or automatically by computer by switching the button from
local to remote position.
Check if the Auto fill function is ON
The balance vessel can also be filled manually with the yellow button Fill (above the balance)
Check if the pressure is applied in the feeding barrel, situated at the backside of the Pilot, for
details refer to chapter B.2.


c) Feeding of heavy hydrocarbons




d) Feeding of gasses (butane)



3. Decoking feeding gasses


The feeding gasses for decoking are situated in the battery at the backside of the reactor.
N2 is fed through the reactor while




4. Preparation of outlet section for a feeding


a) “Turn ON” the TLE1 (if is necessary)



Manual Pilot                                                                                       20
August 2005                                                                             Michael Lottin
b) Switch on the heatings of the exit pipe and sampling systems.
For more information refer to chapter A.2.


c) “Turn ON” the TLE2 and water condenser
TLE2 and water cooler are used to cool down the reactor effluent. In this part heavier HC and
water are condensed and separated
Turn ON the oil pump by pressing the start button
(situated on the pillar nearby pump, “ISKRA DME25” box)
Open red (outlet) and blue (inlet) valves named “koeling” to open the cooling water circuit
Open valve below rotameter “OLIE” to cool the low pressure TLE2
Open valve below rotameter “CONDENSVAT” (if necessary) to cool condenser below TLE2
Open valve below rotameter “ROOKGASSEN” (if necessary) to cool condenser installed
below the high pressure TLE2


d) “Turn ON” the heating of PRV
Switch the temperature controller situated on the temperature control panel on and set
temperature to 150°C.


e) Check the valve setting
For more information refer to chapter B.1.


f) Switch on the water cooler for C4- effluent.
This cooler is used to cool further down the gas samples for the C4- analysis Check the water
level in the “Van der heyden” cooler situated behind the Fisons GC and refill if necessary.
Plug the cooler in.


g) Refill the water absorbers.
Check the colour of the drierite inside the absorbers. If it is pink, refill. If it’s blue it’s OK.


h) Switch on the Lauda cooler.




Manual Pilot                                                                                           21
August 2005                                                                                 Michael Lottin
This is part of the cooling system of the gas samples for the CO-CO2 analysis. Check the
ethanol level in the Lauda bath and refill if necessary. Switch it “ON”. Set point has to be
0°C.


i) Switch "ON" TCD bridges on "Agilent GC" and "Fisons GC".
For more information refer to chapter N


j) Check flame from FI detectors on "Agilent GC" and GCs for C5+ analysis.
For more information refer to chapter N


k) Check whether "GC servers" are switched "ON".


l) Start data acquisition.
For detailed information refer to X-Chrom user guide, chapter K




F. Start cracking experiment

1. Ignition of the flare
The flare should be ignited before the feed of any hydrocarbons!!!
Open the black valve on the yellow tube against the wall
Ignite the flare with a match outside
The flare has to be fed with steam to improve the burning of hydrocarbons present in the
effluent
Therefore put on the steam generator in the cellar
The heating has to be in position 4 and the main switch in position 1
After 45 minutes the green valve can be opened
Open the supply of steam with the big black turning valve against the wall
Check pressure on right manometer (approx. 5 bar)
Flush the water in the steam line with the red valve
Feed the flare with steam by opening the red turning valve
Regulate the pressure on the left manometer to approx. 0.2 bar



Manual Pilot                                                                                 22
August 2005                                                                       Michael Lottin
2. Preparation for cracking experiment
Set temperature profile in Labview
Reset run.nb. in environment sheet in Labview
Switch to cracking position in CO-CO2 sheet in Labview
Start feeding water
Ask André to put on the steam generator in the cellar (main switch has to be put in position
ON and after 45 minutes the green valve has to be opened)
Calibrate CO-CO2 meter
Fully open the effluent-line
Set valves around CO-CO2 meter to cracking positions
Set C4-sample line purge valves (K162 and K161) to position up
Check all gas pressures
Check all the cooling systems
Check the water absorbers and refill if drierite is pink
Ignite the flare outside and feed steam
Open K139 and close K132, K133 and the stand-by valve above TLE2



3. Start cracking experiment
Set the desired water feed in Labview
Start the CO-CO2 logging in Labview
Start the feeding of hydrocarbons
Start the feeding of internal standard (set 70% on channel 1)
Regulate the pressure in the effluent line
Put set point of pressure regulation valve to 0.7 bar (relative pressure)
Close bypass on pressure regulation valve
Switch CO-CO2 meter to the effluent line
Use K150 to regulate pressure on manometer P140 to 0.5 bar
Flowrate through CO-CO2 meter should be approx. 1liter/mim
Use K146 to regulate to 60 on rotameter on top (0.5 bar on P141)
When everything is stable start analyses with first RUN
After every RUN drain the water in the separators by opening the valves K132 and K133
The collector under TLE2 has to be drained with valve K135


Manual Pilot                                                                                 23
August 2005                                                                       Michael Lottin
4. Run analysis. (Do injection.)
a) Start C4- analyses.
Open the valve K151.
Press start on the C4- -button in the environment sheet in labview
By pressing start the sampling system is purged automatically with He for 30”, then for 2’40”
with effluent followed by an injection and again a He purge of 2’40”.
Check whether sample is flowing through sample loops. Therefore check for bubbles in HP
and Fisons gas washing bottle.
After injection close the valve K151.
Status "Acquiring" in Xchrom is expected for channel 1,2 and 3 after 4min.


b) Start C5+ analyses.
Choose a GC, which you are going to use for C5+ analysis.
K125 has to be ‘ON’ to choose GC5, ‘OFF’ to choose GC6.
Choose which Injector you are going to use.
K124 has to be ‘ON’ to choose Inj A (K122), ‘OFF’ to choose Inj B (K123).
Press start on the C5+ -button (Ch5 or Ch6) in the environment sheet in labview
By pressing start the sample loop will be purged with effluent for 60 seconds followed by an
injection
To have this injection at the same time as the automatic injection in C4- section start the C5+
section 3 minutes 35 seconds later in labview
Purge sampling system with He manually by means of opening the valves K110 and K111 on
top of the C5+ sampling system
Status "Acquiring" in Xchrom is expected for channel 5 respectively channel 6


c) Display chromatograms.
In Xchrom Main Window choose ‘View’ and click on ‘Acquiring Data’ to see
chromatograms.



5. Stop cracking experiment
Stop the CO-CO2 logging in Labview
Switch CO-CO2 meter to nitrogen


Manual Pilot                                                                                    24
August 2005                                                                          Michael Lottin
Release the pressure and fully open the effluent line
Fully open K150
Open the blue valve in the middle of the effluent line
Open the bypass of the pressure regulation valve and put setpoint to zero
Stop internal standard feeding
Stop feeding of hydrocarbons
Stop the gas and steam feeding of the flare
When decoking is done the next day set N2 feed to 24.5% to flush out everything
After 30 minutes set N2 to 5% and 10 minutes later to 2% (as low as possible to prevent that
the O2 present in the N2 bottle burns the cokes)
Close in this case also K139 and open K132, K133 and the stand-by valve above TLE2 to
prevent condense entering the effluent line




G. Decoking

1. Preparation for decoking


It is important to start the CO- and CO2-analyser a while before decoking so that the
analysers are well stabilized before using them. For further information refer to chapter I.2.
The ethanol cooler has to be switched on (0 °C)
Switch to decoking position in CO-CO2 sheet in Labview
Switch CO-CO2 meter to nitrogen
Check if effluent line is fully open
Check the water absorber and refill if drierite is pink
Check all gas pressures (air and nitrogen)
Check the cooling system around CO-CO2 meter
Calibrate CO-CO2 meter
Set prestart temperature profile
Feed only nitrogen, no water!! (setpoint on channel 2)




Manual Pilot                                                                                      25
August 2005                                                                            Michael Lottin
2. Start decoking experiment
The total decoking procedure takes approximately 3 hours
(normal decoking time is 100 minutes, elapsed time in CO-CO2 sheet in labview will be 6000)
Decoking is performed by a steam/air mixture.


When temperature profile is reached set valves to decoking positions
For detailed information about valve settings during decoking refer to chapter H.b)
Switch CO-CO2 meter to the effluent
Regulate pressure with K150 (1bar on P140 and 0.5 bar on P141)
The flow through rotameter should be approx. 60
Start the CO-CO2 logging in Labview by pressing the button Decoke scan “ON” in the CO-
CO2 window
Start the feeding of water
When temperatures are stable switch nitrogen to air (setpoint on channel 2)
When CO2 < 1 vol% change the temperature profile
When CO2 < 0.1 vol% stop the feeding of water



3. Stop the decoking experiment
After this period ( = 100 minutes, elapsed time in CO-CO2 in labview has to be 6000 seconds)
stop the CO-CO2 logging
Stop the feeding of air
Change the temperature profile to 500 °C (cell 3 up to cell 7)
Feed 4000g/h water to cool down to 800 °C
Stop the feeding of water
Close K139 and open K132, K133 and the stand-by valve above TLE2



4. Collection of cokes on the filter
Small particles of cokes are collected under TLE by means of a stainless steel filter
After decoking the SS filter has to be taken out of the separator and cleaned with water
The coke is now collected on the coffee filter




Manual Pilot                                                                                       26
August 2005                                                                             Michael Lottin
The weight of the filter after drying (at 105 °C) minus the weight of the filter itself gives us
the amount of collected cokes



H. Sampling system for carbon oxides analysis with IR-analyser.
a) Valve settings during cracking.
Valve K142 has to be closed when all valve settings are done.
Open the grey valve so that the effluent flows through the blue flow meter.
After this flow meter there’s a flow split. A part goes back to the effluent line, therefore open
the grey valve further on this line, the other part goes to the cool section and the water
absorber.
Open valve K149 and the valve above it and close valve K148.
After the water absorber the effluent goes through the black flow meter. Close the valve
above it.
Switch K147 to the left and use valve K146 to regulate the pressure on P141 to 0.5 bar.
Check for bubbles in the CO-CO2 gas washing bottle to see if you have flow through.
For flow measurement the values of the blue flow meter are used.


b) Valve settings during decoking.
Valve K142 has to be closed when all valve settings are done.
Open the grey valve so that the effluent flows through the blue flow meter.
The grey valve further on the effluent line has to be closed now so that there‘s no split flow
here and all the effluent goes through the cool section and the water absorber.
Open valve K149 and the valve above it and close valve K148.
From here the effluent goes through the grey flow meter.
The valve above this flow meter is open now so there’s a flow split here. A part goes back to
the effluent line, the other part goes to the CO-CO2 meter.
Switch K147 to the left and use valve K146 to regulate the pressure on P141 to 0.5 bar.
Check for bubbles in the CO-CO2 gas washing bottle to see if you have flow through.
For flow measurement the values of the grey flow meter are used.




Manual Pilot                                                                                     27
August 2005                                                                           Michael Lottin
I. Calibration procedures

1. How to calibrate C4 --GC’s
a) Purge sample loops with calibration gas.
Choose between two different calibration mixtures by means off the valve under K167
Bottle I: C1-C2
Bottle II: C1-C4
Composition of the bottles can be seen in Appendix 6
Check the pressure in the connected bottle and set output pressure (0.5bar<P<0.8bar).
Valves K161 and K162 have to be in position down
Valve K164 has to be closed
Valve K160 has to be open to check pressure on manometer P160
This pressure can be regulated at 0.5bar with valve K167
Note: higher pressure is dangerous - glass parts are installed


b) Check whether calibration gas is flowing through sample loops.
Check bubbles in the gas washing bottles above GC’s


c) Inject calibration gas.
Press start button situated on "the gas control panel"


d) Wait 4 min and check status of all channels.
"Acquiring" is expected



2. How to calibrate COx analyser (once per day)

Analyser has to be turned on (by power switch on the front panel) at least 4 hours before use
to warm-up
Let flow nitrogen trough the analyser during warming–up
Outlet of analyser has to be connected to atmospheric pressure


a) Feed nitrogen.
Let flow nitrogen trough the analyser


Manual Pilot                                                                                  28
August 2005                                                                        Michael Lottin
On Gas Control Panel open valve Zero-gas CO-CO2
Pressure on P141 has to be 0.5 bar
Open valves K164 (position to black tube), K147 (position to thin tube)
Set outlet flow (0.5 – 1.5 l/min) on rotameter by needle valve K 146
Check pressure on P141 again which has to be 0.5 bar


b) Do zero calibration.
Open valve K164 (position to black tube) in order to feed nitrogen
Press ZERO and CAL on the control panel


c) Do span calibration.
Let flow calibration gas (with concentration of CO ~6 vol. %, CO2 ~3.5 vol. %) through the
analyser. (To set or check the “SPAN value” refer to the analyser manual)
Fully open the valve K 146 (outlet of analyser)
Open calib. bottle
“switch” valve below K167 and K168 to position where calibration bottle is connected
Open valves K161 and K160 to make possible to check inlet pressure (0.5 bar), valve K164
has to be in position to black tube (nitrogen feeding) or closed.
Set pressure 0.5bar on manometer nearby K160 by valve K167
Open valves K164 (position to thin tube), K147 (position to thin tube)
Close K161 to save calibration gas
Set outlet flow (0.5 – 1.5 l/min) on rotameter by needle valve K 146
Wait a while until analyser is purged by cal. gas
Press SPAN select the first component to calibrate by COMP and press CAL
Repeat this for the second component
For details refer to analyser manual
After calibration close cal. bottle and valve K167 and start to feed nitrogen.


Do it in this order to avoid building-up pressure in tubes




Manual Pilot                                                                                29
August 2005                                                                      Michael Lottin
J. Pressure test
a) Valve setting
Close valves K130, K132, K133, K139 and stand-by valve


b) Set reactor under pressure (up to 3 bar) with N2
Set point of MFC behind pilot has to be on 40% (Channel 2 on Brooks)
Switch valve before MFC to N2-side
Open valves K66 and K64
If pressure reaches 3 bar close K66 and K64


c) Pressure has to be stable for at least 1 hour



K. X-Chrom user guide

1. How to prepare X-Chrom
a) Start up X-Chrom software.
Double click blue X-Chrom icon
X-Chrom main window appears


b) Start up X-Chrom software.
Click on “View” and choose “Acquisition status”
In this window you can see status of all connected channels
Only channels 1,2,3,5 and 6 are used
Acq State should be for all channels “Idle”
If not: click on “acquire”, “quit run” and choose “immediately”


c) Prepare all channels for injection.
Set Acq state of all channels at "waiting injection"
Click on channel's row number which you want to set in "waiting position".
In "Acquisition status" window click on "Acquire" and choose "Start run". In displayed
window
as "Project" choose "Pilot"


Manual Pilot                                                                            30
August 2005                                                                  Michael Lottin
as "Instrument" choose "channel x" (x is number of channel).
as "File to use as template" choose last made (datum naming system)
as "Analysis to start" type actual date in following format "yyyymmdd-xx" year, month, day
and variable symbol. (Variable symbol is not obligated)
Confirm by "OK" button and wait till "waiting injection" appear in "Acquisition Status
column".
Repeat this for all 5 channels.


d) Check whether "GC servers" are switched "on".
On-off button at the backside should be on position “I”



2. How to work with X-Chrom
a) Display chromatograms.
Click on "View" and choose "Chromatogram"
The "View Chromatogram" window appears
Choose file name, channel, "pilot” as Project, "All" as Injection and Sample
Confirm by "OK" button and the chromatogram appears


To open an overlay click on “File” and choose “Open Overlay”
The "View Chromatogram" window appears again and you can select a chromatogram to
make an overlay


b) Calculate peak areas for C4- components.
Integrate peaks manually or by means of computer as written below
Click on "Process" and choose "Detect"
Automatic integration is applied for peak detection
Click on "Process" and choose "Identify" to identify peaks


To view peak data calculated by computer click on "View" and choose "Peak Data"
Select in the “Peak View” window the column “Area”
Click on “Edit” and choose “Cut Column”
Click again on “Edit” and choose “Undo Cut Column”


Manual Pilot                                                                                 31
August 2005                                                                       Michael Lottin
The peak data are now on the clipboard and can be pasted in the proper excel file


c) Don't forget to set methane yields in the "Analysis method" for C5+ components.
In the chromatogram click on "File" and choose "Open Analysis"
Put corresponding methane yield (taken from C4--report) into the "Userparameter1" column
Do this for every run, run number is displayed in the first column


d) Calculate peak areas for C5+ components.
Integrate peaks manually by means of an overlay with a previous chromatogram
Or click on "Process" and choose "Detect"
Automatic integration is applied for peak detection
Click on "Process" and choose "Identify" to identify peaks
Check peak identification (Methane first peak, propylene big peak…)
If identification was not successful, then change identification method in "Analysis method"
window (Method Id box)


Click on "Process" and choose "Quantify"
Display results calculated by computer by click on "View" and choose "Peak Data"
Select in the “Peak View” window the columns up to “User Equation 1”
Click on “Edit” and choose “Cut Columns”
Click again on “Edit” and choose “Undo Cut Columns”
The peak data are now on the clipboard and can be pasted in the proper excel file



L. LabView user guide
a) Start up LabView software
Double click the LabView shortcut named pilot_okt2004. Click in the opening window on the
icon RUN (in the upper left corner)
LabView is now started up with as default values all flows zero and all temperatures 400°C


b) Flowsheet window
Here you can set and follow temperature profiles, flow rates and pressures
Data log can be put ON to log all important data


Manual Pilot                                                                                    32
August 2005                                                                          Michael Lottin
Time based scheduling can be enabled or disabled


c) Profile window
Here you can see the temperature profile set versus the current temperature profile


d) Environment window
Here you can start time based scheduling by setting year, day, month, hour and minutes and
pressing OK
Also the analyses for C4- and C5+ section have to be started here


e) CO-CO2 window
Switch the button to ‘Decoke’ or ‘Cracking’ position
To start a ‘scan’ press ‘ON’, to stop it press ‘OFF’
CO-CO2 measurement is in vol%
Effluent flow measurement in ml/min
The blue flow meter is used for cracking
The grey flow meter is used for decoking


f) Burner press window
Here you can see the gas pressures of all burners


g) Service window
Here you can see all activated loop counters


h) Time based scheduling
This can be used to program a certain profile
The profile has to be set in an excel file and has to be saved as text file
The water flow can be set in the column Flow1
In the columns Cell 1 up to Cell 7 the temperatures can be set
The name and location of this file is C:\Users\RDC\Labview\schedule.xls
Switch “enable” ON in the flow sheet
Put the date and time when the profile has to be started in the environment sheet
Auto firing has to be switched ON on the pilot control panel


Manual Pilot                                                                                     33
August 2005                                                                           Michael Lottin
M. Evaluation of results

1. How to calculate calibration factors for C4--GC’s
a) Start EXCEL and open the calib file (with macro enabled).
Path to template E:\Users\pilot\Calib\Calibfile_2003.xls


b) In sheet “bottle I, C1-C2”.
Import peak areas from X-Chrom for each calibration run
Channel 1 = Agilent TCD
Channel 2 = Agilent FID
Channel 3 = Fisons TCD
Compare CF with values from previous calibrations
Check ST DEV


c) In sheet “bottle II, C1-C4”.
Import peak areas from X-Chrom for each calibration run
Channel 1 = Agilent TCD
Channel 2 = Agilent FID
Channel 3 = Fisons TCD
Compare CF with values from previous calibrations
Check ST DEV


d) In sheet “Comparison”.
Copy CF and ST DEV from previous sheets to compare results from bottle I and bottle II



2. How to make report of results C4--analysis
a) Start EXCEL and open the template file (with macro enabled).
Path to template E:\Users\pilot\templates\template_C4min.xls


b) Save file as C4min-yyyymmdd.xls
After saving you can make changes




Manual Pilot                                                                                34
August 2005                                                                      Michael Lottin
c) In sheet “Status”.
Clear all old data by pressing button "Clear all old data"
Press the button “Insert Date”
Fill in manually the cells concerning HC-Feed and Diluent
Press the button “Importing Inj. Status” and choose run number
Press “Import Status”


d) In sheet “CF”
Import         calculated   calibration     factors     from     the   file   with      path
E:\Users\Pilot\Calib\Calibfile_yyyymmdd
In column D for Ch1 and Ch2
In column M for Ch3


e) In sheet “Peak Areas”.
Press the button “Move old” and paste peak areas from X-chrom
(use Cut Column and Undo edit directions)


f) In sheet “Report”.
Print report and press the button “Update results”
Save and repeat this for each run


g) In sheet “Air”
Put parameters about TLE1 airflow
To switch from one run to another press the button “Recalculate Run” and choose run number
in the sheet “Report”



3. How to make report of results C5+-analysis
a) Start EXCEL and open the template file (with macro enabled).
Path to template E:\Users\pilot\templates\template_C5plus.xls


b) Save file as C5plus-yyyymmdd.xls
After saving you can make changes


Manual Pilot                                                                                35
August 2005                                                                      Michael Lottin
c) In sheet “Calcult”.
Clear all old data by pressing button "Clear all old data"
Insert actual date (use required format) and other general data
(sample properties, starting temp,…)
Insert run number
Import data from XChrom (use Cut Column and Undo edit directions)
Press the button “Calculate”
Press the button “Make Report”


d) In sheet “Report”.
Print report


e) In sheet “Calcult”.
Press the button “Update Results”


f) In sheet “List”.
Press the button “Clear list of components”
Press the button “Clear Data”
Paste the list of components in column A
Select the run number in row 3 to sort yields and press the button “Sort Yields”
For the next run press the button “Clear previous imported run” in sheet “Calcult”
Then repeat previous actions




4. How to write final report
a) Start EXCEL and open the template file.
Path to template E:\Users\pilot\templates\template_results.xls


b) Save file as results-yyyymmdd. After saving you can make changes.


c) Clear all old data by pressing button "Clear all old data" in sheet “source Data”.


Manual Pilot                                                                                       36
August 2005                                                                             Michael Lottin
d) In sheet “Condition 1”
Feed, COT (°C) and Date has to be filled in manually


e) In sheet “Source Data”.
Copy following data from sheet “Results” in C4--report:
HC-flow, H2O-flow (dilution will be calculated), temp.profile, pressures, residence time,
Ve/Fo and yields from C4-


f) In sheet “Condition 1”.
Copy data from sheet “list” in C5+-report (only from components witch are not in C4--report)
Paste the names of the components in column B starting from row 14
Paste in column C the Yields and press the button “Calculate Find and Export”
In the following window “Export Run” choose run number and click “Yes”
Start with values from Run1, Run2…
Finally paste Run1 and press “Cancel” when window “Export Run” appears


g) In sheet “Source Data”.
Paste again the names of the components from C5+-report (only from components witch are
not in C4--report) in cell A70, under “Import Yields”
Press the button “Import Yields”
Press the button “Recalculate MB” (press Esc and End to stop the macro if it takes to long)


          Control:    All values in line 579 should be 100
                      Line 38 = line 573
                      Line 39 = line 574
                      …
                      Line 42 = line 578


Press the button “Choose Run to normalize” and choose run number (only use this if mass
balances differ to much from 100%)




Manual Pilot                                                                                   37
August 2005                                                                         Michael Lottin
5. How to make cracking report for CO-CO2
The cracking txt.file logged by process computer can be found in the folder named
E:\Users\Pilot\Main\Decoke
Open this file in excel
The window ‘Text import wizard step 1 of 3’ will be opened
Choose ‘Windows (ANSI)’ as File Origin
Click next (only TAB has to be selected)
Again next and finish
Save this file as cracking-yyyymmdd.xls


Make a chart in a second sheet
Use ‘xy-scatter’ as Chart Type
The first serie is CO (vol%)
The second serie is CO2 (vol%)



6. How to make decoking report for CO-CO2
The decoking txt.file logged by procescomputer can be found in the folder named
E:\Users\Pilot\Main\Decoke
Open this file in excell
The window ‘Tekst import wizard step 1 of 3’ will be opened
Choose ‘Windows (ANSI)’ as File Origin
Click next (only TAB has to be selected)
Again next and finish
Save this file as decoking-yyyymmdd.xls


Make a chart in a second sheet
Use ‘xy-scatter’ as Chart Type
The first serie is CO (vol%)
The second serie is CO2 (vol%)
The third serie shows the amount of cokes in g




Manual Pilot                                                                       38
August 2005                                                             Michael Lottin
N. Basics of GC’s

1. Specifications for C5+-GC’s
a) Type Hewlett Packard 5980 Series II.
Manual available in closet near GC’s


Two GC’s of this type are used for C5+ analysis
Carrier gas is Helium
Column is a capillairy Pona column (length 50m)
Detector is FID (signal on upper GC is approx. 44.5, on lower GC 43.2)
A mixture of Hydrogen and air (1-10) is used as fuel for the flame
Analyse time is approximately 70 min
Temperature programme from -40°C to 250°C
Cooling with liquid Nitrogen


b) Specifications for inlet flows
The flow through the column is 0.65 ml/min
The measured flow at the split vent should be around 215 ml/min
The septum purge flow around 20 ml/min
Increasing the column head pressure will increase the flow through the column which will
lead to smaller retention times


Inlet of different gasses are at the back side of the GC
Yellow tube = Helium: pressure set at 500 kPa
Blue tube = Air: pressure set at 200 kPa
Green tube = Hydrogen: pressure set at 200 kPa


c) Specifications for cooling system
Both GC’s cool as far as possible with air
Therefore give in ambient temperature
Set “Cryo Temp” to 25°C
Set also “Cryo” to ON
This means there’s something else to cool further down, namely liquid nitrogen


Manual Pilot                                                                                39
August 2005                                                                      Michael Lottin
Refill before analyses the dewar for liquid nitrogen


Caution! the risk of burning, for necessary assistance refer to technical personnel


Liquid nitrogen is stored outside. Open the valve of the ranger slowly so that the liquid
nitrogen does not splashes out of the dewar. (A full ranger is approximately 3.5 dewars)
After refilling install the tubing system, valve on it has to be open
Fix the tubing system with the tightening
Close the valve
Turn ON the cryogenic system (Cryoson) situated on the left side of upper GC
Put switchers on “ON“ and “MAINS”
Wait until the red diode detects the ready status (pressure ~0.4bar)


d) Starting and stopping analyses
To start analyses temperature programme has to be started
Press on “Init. Value”, set this to -40°C and confirm with “enter”
GC is ready for injection when the red light is out
At the end of the temperature programme (at 250°C) GC will start to cool down again
To stop analyses “Init. Value” has to be set to 250 °C


e) Temperature program
Inj temp A has to be 250°C
Det temp A 300°C


Init temp               -40 °C
Init time               4 min
Rate                    5 deg/min
Final temp              40 °C
Final time              0 min
Rate A                  3 deg/min
Final temp A            90 °C
Final time A            0 min



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August 2005                                                                           Michael Lottin
Rate B                    8 deg/min
Final temp B              250 °C
Final time B              8 min



2. HP Agilent 6890N GC for C4—section
a) General information
This GC has a FID and two TCD’s. There are five columns and four valves. More
specifications about switching of valves, columns and temperature program can be found in
Appendix 1, Appendix 2 and the GC manual on CD-rom kept by Michael Lottin.
Different methods are already loaded in GC memory:
Method1 and 2 for analyses.
Method3 to put detectors off.
Method4 for activation.
Method8 for night regime.
Method9 is an analyses back-up.


b) Ignition FID
To ignite FID select on the control panel “Back detector”. First set H2 and Air flow on. Then
set flame “ON”.


c) Starting analyses
Load the proper method you want to use. To start analyses press “status” and wait for the
message “ready for injection”. Then press start on the gas control panel.


d) Reactivation of the columns
If separation between the N2, CH4 and the CO peak on Channel 1 is not sufficient the two
molsieves of the Agilent GC have to be regenerated


To take out molsieve 13X column 5 first turn off the front inlet (PP)
This will turn the total H2 flow off
Disconnect the column
First connection at the left is the inlet, first at the right the outlet


Manual Pilot                                                                                  41
August 2005                                                                        Michael Lottin
Connect the column in the Chrompack GC of the Evy installation to regenerate
Second last connection at the left is the inlet, second last at the right the outlet
Apply the He pressure with PR1


To take out molsieve 13X column 3 first put valve 2 in position ON
This will turn off the flow
Disconnect the column
Third connection at the left is the inlet, third at the right the outlet
Connect the column in the Chrompack GC of the Evy installation to regenerate
Fourth connection at the right is the inlet, first at the left the outlet
Apply the He pressure with PR2


Put the column limit to 340 °C, oven init to 320 °C and regenerate the columns during one
night at this temperature



3. Interscience Fisons GC 8340
a) General information
This GC has a TCD, a HayesepN column (2m), a CarbosphereSS column (1.829m)
Carrier gas is He and oven temperature is 60°C
The sample is introduced into the GC with two valves. Those are switched by means of event
1 and event 2. Event 1 has to be ON after 1 second and OFF after 6 minutes. Event 2 has to be
ON after 100 seconds and OFF after 380 seconds.


b) Before analyses.
Start GC up with POWER switch.
Zone1 has to be 110 °C, zone2 has to be 155°C. Check this with the button “actual temp” on
the control panel.
The green lights for ‘Zone power’ and ‘Oven power’ have to be on. If not switch them on
with “Exec”.
Press “Mains” on the TCD control panel. Det temp is set to 15 (= 150°C).
Fil temp has to be set to 21 (= 210 °C). Press “Bridge” so that the green ‘ON’ light is
burning.


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August 2005                                                                            Michael Lottin
c) Starting analyses.
If status is ready (status has to be in ‘Sampling position’), analyses can be started
automatically by pressing the start button in labview.



O. Gas control panel
All pressures and feedings of analytical gases are regulated on this control panel.
Main manometer for nitrogen has to be on approximately 13 bar, for Helium on
approximately 11 bar and for Hydrogen on approximately 8 bar. A detailed scheme of the gas
control panel can be seen in Appendix 4.


a) Applications for nitrogen


         To do zero-calibration of CO-CO2 meter : 1,5 bar
         As carrier gas in Agilent GC (detection of H2) : 7 bar
         To keep pressure in balance vessel for HC : 150 mbar
         To keep pressure in 200 l water barrel : 200 mbar
         As internal standard : 8 bar
         For water pump (mity mite) : 10 bar


b) Applications for helium


         Carrier gas in both C4- GC’s : 10 bar
         Carrier gas in both C5+ GC’s : 8 bar
         Make-up gas Fisons : 10 bar
         C4- sample purge : 2 bar
         C5+ sample purge :


c) Applications for hydrogen


         For FID Agilent : 2,5 bar
         For FID C5+ GC’s : 2,5 bar

Manual Pilot                                                                                     43
August 2005                                                                           Michael Lottin
d) Applications for air


         For FID Agilent : 3 bar
         For FID C5+ GC’s : 3 bar
         To actuators in C4- GC’s : 3 bar




P. Alarm conditions
During the day you have 15 minutes to solve the problem, otherwise the combustion
controller is shut down. At night the combustion controller is shut down immediately.
There are five conditions in which case this is applied:


a) Failing of the exhaust gases venting
This is detected by a contact flow meter (Brooks Shorate 1355 + tube R2-15-A + carboloy
float + inductive alarm 7910). The flow meter has a moveable magnetic coil around its
measurement tube. When the float comes into the coil, it gives an electrical disturbance which
after amplification switches a contact of the alarm current cycle.
The light “ VACUUMPOMP “on the pilot control panel will be burning.




b) Flame deflection
In this case the light “Brander UIT” on the Pilot control panel will be burning.
In the exhaust gas channel of each cell, a venting pipe is installed. The exhaust gases are
purged via a methane sensitive sensor (model 780) and a flow rate regulator (Brooks Sho-rate
1350). The gas flow rate through the sensor is set on 2 l/min. The seven pipes come together
in a common flow rate regulator (Brooks Sho-rate 1355 + tube R6-15-A + SS-float) which is
on his turn connected to a vacuum pump. In the Sieger alarm box (model 5700) the signal of
the sensors is amplified. While all burners are working, the zero level of the amplifiers is set.
The alarm level is regulated such that one flame deflection of the twelve burners is enough to
cause an alarm. In case of a deflection of a burner, an excess of unburned gas is detected by




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August 2005                                                                           Michael Lottin
one of the sensors. After amplifying the signal, the contact will switch and interrupt the alarm
current cycle.


c) Back-fire
In the 7 cells of the furnace, the burner feeding pipe is equipped with a back-fire valve. In
case of back-fire, the flame in such a valve heats up a locally bi-metal which extends and
closes via a mechanical coupling the valve as well switches the electrical contact. This contact
also takes part of the alarm current cycle.
The light on the pilot control panel “ CEL VLAM<< “ of the proper cell will be burning.


d) High and low natural gas pressure
The gas feeding pressure of the burner regulator has to be between 10 cm w.c. and 25 cm w.c.
When the pressure is too high or too low, the contact of the membrane sensors will interrupt
the alarm current cycle (Mercoid Diaphragm control).
The light “GASDRUK HOOG” or “GASDRUK LAAG” on the pilot control panel will be
burning.


e) Over heating reactor
If one of the thermocouples in the oven reaches a temperature higher than 950°C, a contact
will switch and interrupt the alarm current cycle.




f) High pressure at inlet reactor
Two safety manometers, P21 and P50, verify the pressure at the reactor inlet.
They are situated at the left of the main control panel.
Both are set at 5 bar and control the magnetic valves M21 and M50
If the pressure exceeds this value the magnetic valves will close
M21 closes hereby the feeding line of nafta / liquid hydrocarbons
M50 closes the feeding line of butane / gas hydrocarbons




Manual Pilot                                                                                    45
August 2005                                                                          Michael Lottin
Q. Appendix 1
Separation specifications Agilent GC.


 Component        Component      Carrier   Separation Separation            Detection
   formula           name         gas      Channel 1 Channel 2     TCD 1   TCD 2          FID
H2             hydrogen           N2           1          -          +       -             -
N2             nitrogen           He           6          -          -       +             -
CH4            methane            He           7          1          -       +             -
               carbon
CO             monoxide            He          8          -          -        +             +
CO2            carbon dioxide      He          2          -          -        +             -
C2H6           ethane              He          4          2          -        +             +
C2H4           ethylene            He          3          3          -        +             +
C2H2           acetylene           He          5         10          -        +             +
C3H8           propane             He          -          4          -        -             +
C3H6           propylene           He          -          6          -        -             +
cyC3H6         cyclopropane        He          -          5          -        -             +
C3H4 (PD)      propadiene          He          -          9          -        -             +
C3H4
(MEAC)         methylacetylene     He          -         18          -        -             +
iC4H10         iso-butane          He          -          7          -        -             +
nC4H10         n-butane            He          -          8          -        -             +
1C4H8          1-butene            He          -         12          -        -             +
iC4H8          iso-butene          He          -         13          -        -             +
cis-2-C4H8     cis-2-butene        He          -         14          -        -             +
trans-2-
C4H8           trans-2-butene      He          -         11          -        -             +
1,3-C4H6       1,3-butadiene       He          -         17          -        -             +
iC5H12         iso-pentane         He          -         15          -        -             +
nC5H12         n-pentane           He          -         16          -        -             +

No. of
column                   type                L [m]     D [mm]      Flow [cm³/min]    max. T [°C]
       1           HP-5 Pre-column            5?        0,53             5,2            300
       2         HP-PLOT AI2O3 - S25          50        0,53             5,2            200
       3          Molecular Sieve 13X          3          3                             350
       4              Porapack N               3          3                             190
       5          Molecular Sieve 13X         6ft         3                             350




Manual Pilot                                                                                    46
August 2005                                                                         Michael Lottin
R. Appendix 2
Settings Agilent GC.


  Swiching of        Valve 1       Valve 2          Valve 3      Valve 4    Valve 5     Valve 6
                                                      C2           C4
   time [min]      H2 injection    PG trap         injection    injection      ?        TCD 1-2   FD polarity
     default            off          off               off          off        |          off          on
          0.01           |            |                 |            |         |          on            |
          0,10          on            |                on           on         |           |            |
          1,20          off           |                 |            |        off         off          off
          1,30           |            |                 |           off        |           |            |
          3,90           |           on                 |            |         |           |            |
         10,00           |           off               off           |         |           |            |
                                                                                       TCD 1 -    neg.
ON - position injection           holding     injection        injection       ?       ON         polarity
OFF -                                                                                  TCD2 -     positive
position      backflush           analysing backflush          backflush       ?       ON         pol.

                         temperature program
holding                           40°C                           4min
heating               form 40 to 170°C (10°C/min)                13min
holding                          170°C                           5min

Necessary Inlet pressures to the GC - Agilent
Gas           Used for              Pressure [Bar]              regulator   location
H2               FID                          5                     3        front
He               carrier                      6                     1        back
N2               carrier                      5                     5        back
Air              FID                          5                     6        back
Air              actuators                   2,5                    7        front




Manual Pilot                                                                                             47
August 2005                                                                                   Michael Lottin
S. Appendix 3
Decoking conditions after ethane cracking.


                  Fwater    Fair    Fnitrogen   Cell 3   Cell 4   Cell 5   Cell 6       Cell 7
                  (g/s)    (Nl/s)   (Nl/s)      (°C)     (°C)     (°C)     (°C)          (°C)

Pre Start          0.28      0       0.23        750      800      800      800          800

Start              0.28    0.23        0         750      800      800      800          800


CO2<1 vol>%        0.28    0.23        0         750      900      900      900          900


CO2<0.1 vol>%       0      0.23        0         750      900      900      900          900




Manual Pilot                                                                                    48
August 2005                                                                         Michael Lottin
T. Appendix 4
Detailed scheme gas control panel.




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August 2005                          Michael Lottin
U. Appendix 5




Manual Pilot               50
August 2005     Michael Lottin
V. Appendix 6
Bottle I contents:


                       vol %      mol. gew

H2                      18,3          2
CO2                      3,5         44
C2H4                    29,7         28
C2H6                     3,3         30
C2H2                     1,4         26
N2                      12,6         28
CO                       5,9         28
CH4                     25,3         16

                        100


Bottle II contents:


                       vol %       mol. wt

H2                    12,6300    2,0159518
CO2                   0,0556     44,0096463
N2                    14,2300    28,0134462
CO                    0,2610     28,0103416
CH4                   25,3628    16,0429405
C2H6                  3,4200     30,0699292
C2H4                  22,7700    28,0539774
C3H8                  0,1834     44,0969179
C3H6                  12,1100    42,0809661
iC4H10                0,1206     58,1239066
nC4H10                0,2517     58,1239066
1.2 C3H4              0,1900     40,0650143
C2H2                  0,5300     26,0380256
tr2C4H8               0,2148     56,1079548
1C4H8                 0,8400     56,1079548
iC4H8                 1,0400     56,1079548
c2C4H8                0,2081     56,1079548
1.3C4H6               4,7800     54,092003
1 C3H4                0,8020     40,0650143

                      100,0000




Manual Pilot                                             51
August 2005                                   Michael Lottin

				
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