Experimental operation of the unit

After catalyst charging and the flow vs. RPM measurement is done, the reactor should be closed and flushed out with nitrogen while the impeller runs, until O2 drops below a few tenths of a percent. Then a static pressure and leak test should be made by turning off the forward pressure controller and the flow controller. If an observable drop of pressure occurs within 15 minutes, all joints and connections should be checked for leaks and fixed before progressing any fijither. 

With all leaks stopped, and the reactor under test pressure with nitrogen, set the nitrogen pressure regulator to the lowest pressure on the controller, but above 0.3 atmosphere or 5 psig. Now open the flow controller and set the N2 flow to 66 mL/s, equivalent to 10.5 mols/hr rate, to start the flow. Also start heating the unit. 

To open the reactor for inspecting or changing the catalyst, extreme caution must be used. A used catalyst is completely reduced and has some methanol and other combustibles adsorbed on the surface. The used catalyst can heat up when exposed to air and even ignite. A catalyst overheated this way is not useful for further studies and a burned-down laboratory is not useful at all. 

The proper method to remove the catalyst involves stabilization. The method for this is usually recommended by the catalyst manufacturer. With the reactor still closed, cold and flushed with nitrogen, admit nitrogen with less than 1 % oxygen in it, while the impeller is running. This oxidizes the organics and the metallic surface of the catalyst under well-controlled conditions after which the catalyst can be exposed to air without danger of overheating. 

All equipment should be used according to manufacturer s specifications and in compliance with all applicable regulations. 

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