Quick Guide :
A. Preparation and checking procedures (a few days before experiment)
1. Check the installation.
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".
2. Check the heatings.
a) Switch on the temperature console.
b) Test the heating of the effluent line and the sampling pipes for the C4- analysis.
c) Test the heating of the sampling pipes for the C5+ analysis.
d) Test the heating of the C5+ oven.
e) Test the heating of the pressure regulation valve.
f) Test the heating of the heavy HC feeding system.
3. Analysis part preparation
a) Check amount of analytical gases.
b) Order liquid nitrogen needed for C5+ analysis.
c) Check amount of calibration gases (HC calibration mixtures).
d) Check amount of the nitrogen used as internal standard.
e) Check function of GCs for the C5+ analysis.
f) Do calibration of GCs for the C4- analysis.
4. Check the sampling system.
a) Test whether C4- sample loops are free.
b) Check cleanness and permeability of C5+ sample loops
5. Find setting parameters.
B. Check vessels and valve setting before experiment.
1. Set and check valves position.
a) Check whether the valve K150 is fully open. If not open it.
b) Check whether the valve K151 is closed. If not, close it.
c) Prepare the IR sampling system for carbon oxides analysis.
d) Check whether valves K142, K138, K137 and 139 are open. If not open them.
e) Check whether valves K131 and K134 are closed. If not close them.
f) Check whether valves K132 and K133 are closed. If not close them.
g) Check whether the valve K105 is open. If not open it.
h) Close the valve K130.
i) Prepare the C4- injection system.
j) Prepare the C5+ injection system.
k) Connect or disconnect TLE1.
2. Fill up all operational vessels, which you are going to use.
a) Apply overpressure to storage barrels (max. 0.2bar).
b) Feed the water operational storage vessel.
c) Feed the naphtha operational storage vessel.
d) Feed the operational storage vessel for heavy HC.
e) Feed the operational storage vessel for liquefied HC gases.
f) Check the battery for feeding HC gases
g) Check the bottles with gas used to decoke
h) Check the storage amount of all another liquids and gases necessary for experiment.
C. Heating-up of the furnace
1. Start-Up the reactor
a) Preparation.
b) Heating up (three persons are required).
c) Resetting of SIEGER alarm cupboard
2. Operation during the day or night
a) Operation during the day
b) Operation during the night
D. Cooling down and shut down of the reactor
E. Feeding
1. Feeding system preparation.
a) Water feeding.
b) Feeding of the internal standard (N2) at the reactor output.
c) Combustion controller
d) heat-up the “butane” line (if necessary).
e) heat-up the heavy HC feeding section (if necessary).
f) apply pressure in all storage vessels which are going to be used
g) Prepare vessels for naphtha, water and heavy HC.
h) Check amount of nitrogen used as the overpressure gas for feeding of liquids.
2. Hydrocarbon feeding systems
a) Feeding of liquefied gasses
b) Feeding of liquid hydrocarbons
c) Feeding of heavy hydrocarbons
d) Feeding of gasses (butane)
3. Preparation of outlet section for a feeding
a) “Turn ON” the TLE1 (if is necessary)
b) Switch on the heatings of the exit pipe and sampling systems.
c) “Turn ON” the TLE2 and water condenser
d) “Turn ON” the heating of PRV
e) Check the valve setting
f) Switch on the water cooler for C4- effluent.
g) Refill the water absorbers.
h) Switch on the Lauda cooler.
i) Switch "ON" TCD bridges on "Agilent GC" and "Fisons GC".
j) Check flame from FI detectors on "Agilent GC" and GCs for C5+ analysis.
k) Check whether "GC servers" are switched "ON".
l) Start data acquisition.
F. Start cracking experiment
1. Ignition of the flare
2. Preparation for cracking experiment
3. Start cracking experiment
4. Run analysis. (Do injection.)
a) Start C4- analyses.
b) Start C5+ analyses.
c) Display chromatograms.
5. Stop cracking experiment
G. Decoking
1. Preparation for decoking
2. Start decoking experiment
3. Stop the decoking experiment
4. Collection of cokes on the filter
H. Sampling system for carbon oxides analysis with IR-analyser.
a) Valve settings during cracking.
b) Valve settings during decoking.
I. Calibration procedures
1. How to calibrate C4 --GC’s
a) Purge sample loops with calibration gas.
b) Check whether calibration gas is flowing through sample loops.
c) Inject calibration gas.
d) Wait 4 min and check status of all channels.
2. How to calibrate COx analyser (once per day)
a) Feed nitrogen.
b) Do zero calibration.
c) Do span calibration.
J. Pressure test
a) Valve setting
b) Set reactor under pressure (up to 3 bar) with N2
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.
b) Start up X-Chrom software.
c) Prepare all channels for injection.
d) Check whether "GC servers" are switched "on".
2. How to work with X-Chrom
a) Display chromatograms.
b) Calculate peak areas for C4- components.
c) Don't forget to set methane yields in the "Analysis method" for C5+ components.
d) Calculate peak areas for C5+ components.
L. LabView user guide
a) Start up LabView software
b) Flowsheet window
c) Profile window
d) Environment window
e) CO-CO2 window
f) Burner press window
g) Service window
h) Time based scheduling
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).
b) In sheet “bottle I, C1-C2”.
c) In sheet “bottle II, C1-C4”.
d) In sheet “Comparison”.
2. How to make report of results C4--analysis
a) Start EXCEL and open the template file (with macro enabled).
b) Save file as C4min-yyyymmdd.xls
c) In sheet “Status”.
d) In sheet “CF”
e) In sheet “Peak Areas”.
g) In sheet “Air”
3. How to make report of results C5+-analysis
a) Start EXCEL and open the template file (with macro enabled).
b) Save file as C5plus-yyyymmdd.xls
c) In sheet “Calcult”.
d) In sheet “Report”.
e) In sheet “Calcult”.
f) In sheet “List”.
4. How to write final report
a) Start EXCEL and open the template file.
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”.
d) In sheet “Condition 1”
e) In sheet “Source Data”.
f) In sheet “Condition 1”.
g) In sheet “Source Data”.
5. How to make cracking report for CO-CO2
6. How to make decoking report for CO-CO2
N. Basics of GC’s
1. Specifications for C5+-GC’s
a) Type Hewlett Packard 5980 Series II.
b) Specifications for inlet flows
c) Specifications for cooling system
d) Starting and stopping analyses
e) Temperature program
2. HP Agilent 6890N GC for C4—section
a) General information
b) Ignition FID
c) Starting analyses
d) Reactivation of the columns
3. Interscience Fisons GC 8340
a) General information
b) Before analyses.
c) Starting analyses.
O. Gas control panel
a) Applications for nitrogen
b) Applications for helium
c) Applications for hydrogen
d) Applications for air
P. Alarm conditions
a) Failing of the exhaust gases venting
b) Flame deflection
c) Back-fire
d) High and low natural gas pressure
e) Over heating reactor
f) High pressure at inlet reactor
Q. Appendix 1
R. Appendix 2
S. Appendix 3
T. Appendix 4
U. Appendix 5
V. Appendix 6
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 chapterJ
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.
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 theC5+ 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 thepressure regulation valveis regulated by the‘temperature controller’ situatedon 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.
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 standardis 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) Testwhether 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 Fout! Verwijzingsbron niet gevonden.
Connecta bottle withpressurised 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 bottlesfor 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.
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 K167and 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. K122has to be ‘OFF’, in purging position. Check bubbles in the gas washing bottle above the C5+ 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.)
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 controlabove 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.
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.
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.