Quick guide - UGent personal websites



Quick Guide :

A. Preparation and checking procedures (a few days before experiment) 7

1. Check the installation. 7

a) Check whether all pipes and vessels are clean. 7

b) Check whether all valves are clean and functional. 7

c) Check whether all parts are installed properly. 7

d) Do the "pressure-test". 7

2. Check the heatings. 7

a) Switch on the temperature console. 7

b) Test the heating of the effluent line and the sampling pipes for the C4- analysis. 7

c) Test the heating of the sampling pipes for the C5+ analysis. 8

d) Test the heating of the C5+ oven. 8

e) Test the heating of the pressure regulation valve. 8

f) Test the heating of the heavy HC feeding system. 8

3. Analysis part preparation 8

a) Check amount of analytical gases. 8

b) Order liquid nitrogen needed for C5+ analysis. 9

c) Check amount of calibration gases (HC calibration mixtures). 9

d) Check amount of the nitrogen used as internal standard. 9

e) Check function of GCs for the C5+ analysis. 9

f) Do calibration of GCs for the C4- analysis. 9

4. Check the sampling system. 9

a) Test whether C4- sample loops are free. 9

b) Check cleanness and permeability of C5+ sample loops 10

5. Find setting parameters. 10

B. Check vessels and valve setting before experiment. 10

1. Set and check valves position. 10

a) Check whether the valve K150 is fully open. If not open it. 10

b) Check whether the valve K151 is closed. If not, close it. 11

c) Prepare the IR sampling system for carbon oxides analysis. 11

d) Check whether valves K142, K138, K137 and 139 are open. If not open them. 11

e) Check whether valves K131 and K134 are closed. If not close them. 11

f) Check whether valves K132 and K133 are closed. If not close them. 11

g) Check whether the valve K105 is open. If not open it. 11

h) Close the valve K130. 11

i) Prepare the C4- injection system. 11

j) Prepare the C5+ injection system. 12

k) Connect or disconnect TLE1. 12

2. Fill up all operational vessels, which you are going to use. 12

a) Apply overpressure to storage barrels (max. 0.2bar). 12

b) Feed the water operational storage vessel. 12

c) Feed the naphtha operational storage vessel. 12

d) Feed the operational storage vessel for heavy HC. 13

e) Feed the operational storage vessel for liquefied HC gases. 13

f) Check the battery for feeding HC gases 13

g) Check the bottles with gas used to decoke 13

h) Check the storage amount of all another liquids and gases necessary for experiment. 13

C. Heating-up of the furnace 14

1. Start-Up the reactor 14

a) Preparation. 14

b) Heating up (three persons are required). 14

c) Resetting of SIEGER alarm cupboard 15

2. Operation during the day or night 15

a) Operation during the day 15

b) Operation during the night 16

D. Cooling down and shut down of the reactor 16

E. Feeding 17

1. Feeding system preparation. 17

a) Water feeding. 17

b) Feeding of the internal standard (N2) at the reactor output. 17

c) Combustion controller 17

d) heat-up the “butane” line (if necessary). 18

e) heat-up the heavy HC feeding section (if necessary). 18

f) apply pressure in all storage vessels which are going to be used 18

g) Prepare vessels for naphtha, water and heavy HC. 18

h) Check amount of nitrogen used as the overpressure gas for feeding of liquids. 18

2. Hydrocarbon feeding systems 19

a) Feeding of liquefied gasses 19

b) Feeding of liquid hydrocarbons 19

c) Feeding of heavy hydrocarbons 19

d) Feeding of gasses (butane) 19

3. Preparation of outlet section for a feeding 19

a) “Turn ON” the TLE1 (if is necessary) 20

b) Switch on the heatings of the exit pipe and sampling systems. 20

c) “Turn ON” the TLE2 and water condenser 20

d) “Turn ON” the heating of PRV 20

e) Check the valve setting 20

f) Switch on the water cooler for C4- effluent. 20

g) Refill the water absorbers. 20

h) Switch on the Lauda cooler. 20

i) Switch "ON" TCD bridges on "Agilent GC" and "Fisons GC". 21

j) Check flame from FI detectors on "Agilent GC" and GCs for C5+ analysis. 21

k) Check whether "GC servers" are switched "ON". 21

l) Start data acquisition. 21

F. Start cracking experiment 21

1. Ignition of the flare 21

2. Preparation for cracking experiment 22

3. Start cracking experiment 22

4. Run analysis. (Do injection.) 23

a) Start C4- analyses. 23

b) Start C5+ analyses. 23

c) Display chromatograms. 23

5. Stop cracking experiment 23

G. Decoking 24

1. Preparation for decoking 24

2. Start decoking experiment 25

3. Stop the decoking experiment 25

4. Collection of cokes on the filter 25

H. Sampling system for carbon oxides analysis with IR-analyser. 26

a) Valve settings during cracking. 26

b) Valve settings during decoking. 26

I. Calibration procedures 27

1. How to calibrate C4 --GC’s 27

a) Purge sample loops with calibration gas. 27

b) Check whether calibration gas is flowing through sample loops. 27

c) Inject calibration gas. 27

d) Wait 4 min and check status of all channels. 27

2. How to calibrate COx analyser (once per day) 27

a) Feed nitrogen. 27

b) Do zero calibration. 28

c) Do span calibration. 28

J. Pressure test 28

a) Valve setting 28

b) Set reactor under pressure (up to 3 bar) with N2 29

c) Pressure has to be stable for at least 1 hour 29

K. X-Chrom user guide 29

1. How to prepare X-Chrom 29

a) Start up X-Chrom software. 29

b) Start up X-Chrom software. 29

c) Prepare all channels for injection. 29

d) Check whether "GC servers" are switched "on". 30

2. How to work with X-Chrom 30

a) Display chromatograms. 30

b) Calculate peak areas for C4- components. 30

c) Don't forget to set methane yields in the "Analysis method" for C5+ components. 31

d) Calculate peak areas for C5+ components. 31

L. LabView user guide 31

a) Start up LabView software 31

b) Flowsheet window 31

c) Profile window 32

d) Environment window 32

e) CO-CO2 window 32

f) Burner press window 32

g) Service window 32

h) Time based scheduling 32

M. Evaluation of results 33

1. How to calculate calibration factors for C4--GC’s 33

a) Start EXCEL and open the calib file (with macro enabled). 33

b) In sheet “bottle I, C1-C2”. 33

c) In sheet “bottle II, C1-C4”. 33

d) In sheet “Comparison”. 33

2. How to make report of results C4--analysis 33

a) Start EXCEL and open the template file (with macro enabled). 33

b) Save file as C4min-yyyymmdd.xls 33

c) In sheet “Status”. 34

d) In sheet “CF” 34

e) In sheet “Peak Areas”. 34

g) In sheet “Air” 34

3. How to make report of results C5+-analysis 34

a) Start EXCEL and open the template file (with macro enabled). 34

b) Save file as C5plus-yyyymmdd.xls 34

c) In sheet “Calcult”. 35

d) In sheet “Report”. 35

e) In sheet “Calcult”. 35

f) In sheet “List”. 35

4. How to write final report 35

a) Start EXCEL and open the template file. 35

b) Save file as results-yyyymmdd. After saving you can make changes. 35

c) Clear all old data by pressing button "Clear all old data" in sheet “source Data”. 35

d) In sheet “Condition 1” 36

e) In sheet “Source Data”. 36

f) In sheet “Condition 1”. 36

g) In sheet “Source Data”. 36

5. How to make cracking report for CO-CO2 37

6. How to make decoking report for CO-CO2 37

N. Basics of GC’s 38

1. Specifications for C5+-GC’s 38

a) Type Hewlett Packard 5980 Series II. 38

b) Specifications for inlet flows 38

c) Specifications for cooling system 38

d) Starting and stopping analyses 39

e) Temperature program 39

2. HP Agilent 6890N GC for C4—section 40

a) General information 40

b) Ignition FID 40

c) Starting analyses 40

d) Reactivation of the columns 40

3. Interscience Fisons GC 8340 41

a) General information 41

b) Before analyses. 41

c) Starting analyses. 42

O. Gas control panel 42

a) Applications for nitrogen 42

b) Applications for helium 42

c) Applications for hydrogen 42

d) Applications for air 43

P. Alarm conditions 43

a) Failing of the exhaust gases venting 43

b) Flame deflection 43

c) Back-fire 44

d) High and low natural gas pressure 44

e) Over heating reactor 44

f) High pressure at inlet reactor 44

Q. Appendix 1 45

R. Appendix 2 46

S. Appendix 3 47

T. Appendix 4 48

U. Appendix 5 49

V. Appendix 6 50

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.

1 Check whether all pipes and vessels are clean.

2 Check whether all valves are clean and functional.

3 Check whether all parts are installed properly.

4 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.

1 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).

2 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.

3 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

4 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.

5 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.

6 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

1 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

2 Order liquid nitrogen needed for C5+ analysis.

Ask Michael to order liquid nitrogen. A full ranger is approximately 3.5 vessels.

3 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.

4 Check amount of the nitrogen used as internal standard.

Internal standard is taken from the battery outside. Check pressure on the gas control panel.

5 Check function of GCs for the C5+ analysis.

Inject the mixture from the bottle with the calibration mixture for the FID calibration.

6 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.

1 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 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 ................
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