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Appendix A: Start up, Running, and Shut Down Procedure 1. Turn chiller on and set to 0ooC (45 mins to cool to target temperature) 2. Power switch is in the back and controller 3. Check cooling fluid has enough liquid 4. Fill methanol collection vials (large vials: 100 grams, small vials: 50 grams) and hook up the vials in series to the exit stream of system. 5. Record exact weights of the empty vials and the vials containing methanol before hooking up to system for collection. 6. Fill reactor vessel with butanol/water solution, measure concentrations (1-3 wt%), *MAKE SURE VESSEL LINES ARE CLOSED (valve below vessel should be perpendicular to line) 7. Attach reactor vessel to system with clamps 8. Check O-RING before/after each run 9. Wires connected to the reactor unit should point towards the sugar water vessel (towards the back right side of the system when looking from the front side) - this makes it easier to secure the heating jacket 10. Tighten nut above valve (use fingers first to make sure the thread isn’t slipping) 11. Wrap heating jacket around vessel - tie strings 12. Turn heating jacket (40oC) and heating line tapes (60oC) on. Put stirrer on (flip motor switch to III). 13. Turn on CO2, watch leftmost gauge (pressure of tank - should stay at about 900PSI) 14. Around back, turn valve for CO2 open slightly to purge line, for about 5 seconds. (wait for gurgle sound in line) Close valve after purge step is complete. 15. Open the two valves below the reactor and the value at the top of the reactor. 16. Turn on the pumps (Watch for bubbles in the view cell. Middle gauge needle should tick with sounds). 17. Wait for pressure to reach 1500 PSI on the main pressure gauge above reactor and start timer for run when a substantial stream of gas is flowing through the methanol filled collection vessels. Now use Wet test meter to monitor the gas flow rate during the run. 18. Switch samples every (10-15) minutes. *CHECK FOR FROZEN PIPES (could cause surging in the exit stream) Shut off (Emergency): 1. Turn off pumps to stop build up of pressure 2. Turn off CO2 supply 3. Depressurize the column. 4. There are two valves connected to the reactor that are used for depressurization. Use the one with the attached metal pipe to collect any exiting fluid in a sampling container near base of system. 5. ***Release pressure very slowly. If gas is released too quickly, the pipes will freeze over, causing blockages. Change valve release point when first valve snows over and no fluid is exiting system. 66PDF Image | Extraction of Bio-Butanol using Supercritical Carbon Dioxide
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