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1 Standard Operating Procedure Inert Gas/Vacuum Schlenk Line John Standard Operating Procedure Inert Gas/Vacuum Schlenk Line John Hodul, February 2019 Description of Process The inert vacuum lines located in fume hoods 1,2, and 3 in FRNY 2182 require special training in order to use them. These pieces of equipment are used for removing oxygen and water from reaction vessels with nitrogen (N2) or Argon (Ar) via purge/refilling or freeze-pump-thaw techniques. Required Training Purdue School of Chemical Engineering Safety Orientation P.O.W.E.R. Lab safety orientation (including fume hood induction) Engineering and Ventilation Controls The schlenk lines are located inside of fume hoods one and two in FRNY 2182. Ensure that while working in the fume hoods (regardless of whether it contains a vacuum line) the sash is at least at the minimum working height! This minimizes exposure to the chemicals as well as projectiles from explosion/implosion of vacuum line vessel in case of breach. Personal Protective Equipment (while using fume hood/vacuum line) EYE PROTECTION: Safety glasses (or face shield if desired) PROTECTIVE CLOTHING: Laboratory coat, gloves (nitrile/neoprene), for freeze-pump-thaw use cryo gloves (orange gloves located above the oven) ENGINEERING CONTROL: Keep hood sash at the minimum working height. NEVER raise the sash above this level if there is any reaction in the hood. 1 Use of the Schlenk Line 1. Ensure that the vacuum pump is on (the switch is located on the back of the pump, which is in the cabinet under the hood), the cabinet door is open, and the compressed cylinder gas is not empty (i.e., the regulator supply pressure to the desired fumehood is 0.5 bar at all times, refer to Appendix 2 & 3). 2. Verify that there is an open port with red thick walled tubing on the Schlenck line (refer to Appendix 4) available for use. If there is not a line, add a line if there is an open port. Be certain to use the appropriate connector, O-ring, and clamp. 3. Once you have identified an open spot, use the red thick walled rubber tubing to connect the Schlenck line to the reaction flask. a. Connect the red tubing to the reaction flask. b. Ensure that there is a good seal at all joints. Use vacuum grease, keck clamps, rubber septum (that are folded over completely), stopcocks, and zip ties to ensure there are no leaks. 4. Before touching the vacuum or purging valves on the Schlenck line ensure that ALL other lines are closed (i.e., ALL black valves are finger tight clockwise). This is to prevent tampering with any other reaction taking place at that time. 5. Vacuum line operation a. Check that the reaction flask is properly set up and sealed as indicated in step 3. b. To open the reaction flask to vacuum open the top valve on the Schlenck line by turning the valve counter clockwise; no other line should be open at this time. The pressure reading on the regulator will increase and then pump down, indicating the valve is open. c. At this point, the valve between the flask and the vacuum line should be closed. As such, the pressure should drop quickly. If it does not, there is a leak between the vacuum line and the valve. If there is no leak, open the valve to the reaction flask. d. The pressure should decrease to <0.5 Torr within minutes of opening valve; timing will depend on size of reaction flask. If the pressure does not decrease, there is a leak in the setup. Check that every connection is properly sealed and try again. e. Once the pressure has reached the desired level (always < 0.5 Torr), turn off vacuum by closing the valve on the Schlenck line: turn the valve clockwise finger tight. 6. Inert gas line operation a. Check that the reaction flask is properly set up and sealed as indicated in step 3. b. Before opening the inert gas line to the reaction flask, open the inert gas line that is not currently being used. This will vent the system; if the line has not been used for several days there can be a pressure build up in the line and can result in over- 2 pressurizing of the reaction flask. Also, this is the proper time to ensure that the compressed gas cylinder is not empty. At this time the flow of gas can also be adjusted, this is achieved by adjusting the flow meter (refer to Appendix 4) to the desired setting. c. To purge or refill the reaction flask, open the bottom valve on the Schlenck line by turning the valve counter clockwise. i. If you are refilling a vessel, open the valve for only 2-3 seconds. This is to avoid over-pressurizing the vessel. ii. If you are purging a vessel, after opening the inert gas line immediately, attach a bubbler through the rubber septum (refer to Appendix 4). d. To turn off the inert gas flow, turn valve clockwise finger tight. 7. Liquid nitrogen operation for freeze-pump-thaw cycle: a. Fill the portable dewar from the large liquid nitrogen (LN2) tanks behind the glovebox. b. In the small round dewar add LN2 and insert reaction flask (refer to Appendix 5). c. Once the solution is frozen, pull vacuum on the vessel with the solution still in the dewar. Ensure that the solution is COMPLETELY frozen before pulling vacuum. Ensure that the flask remains submerged in LN2 while pulling vacuum. d. Once the pressure has decreased to the desired pressure, close the vacuum line valve, and insert reaction flask in a water bath to thaw the solution. Closing the valve prior to thawing is a critical step; do not overlook it. Otherwise, solvent will get pulled in the vacuum and damage parts. You should see evolution of gas that was trapped in the frozen solid escaping during the thawing process. e. Repeat part b-d three times. f. After the last thaw cycle refill the vessel with inert gas. For this, follow step 6. 8. Vacuum Distillation process (refer to Appendix 6).: a. Fill the vacuum trap dewar completely with liquid nitrogen. NEVER let the liquid nitrogen level fall below 50%! b. Clamp the vacuum distillation head over the oil bath, apply vacuum grease to the round bottom flask connections, and attach the liquid round bottom flask (RBF) to the 45º connection with a stir bar. Clamp the clean receiving distillate RBF to the other connection (below the condenser). Ensure that both of these connections are (yellow) clamped and there is a complete vacuum grease seal at each connection. c. Generously grease the thermometer and insert it into the side of the distillation column, ensuring that there is a complete vacuum grease seal at each connection. d. Attach the inlet condenser line to the bottom condenser sidearm and the outlet condenser line to the top of the condenser sidearm. Screw in place tightly and test connections to detect any leaks (the condenser line is the two top most connections). e. Attach the vacuum line firmly to the vacuum port sidearm of the distillation head (the vacuum line is the bottom most connection). f. Immerse the liquid containing RBF into the oil bath and turn on the stirring on the hotplate until there is gentle mixing inside the RBF. 3 g. Gradually open the attached vacuum line on the distillation head and make note of the pressure that the vacuum line gauge reads. Monitor closely the bubbling of the liquid inside the oil bath immersed RBF to ensure the liquid does not 'bump' inside the column and up the distillation head. h. Gradually keep opening the vacuum line to achieve the sufficient vacuum pressure for distillation. Watch for distillate coming over into the receiving RBF. i. If required, gradually increase the temperature in the oil bath to achieve desired separation. Note the thermometer reading gives the temperature of the distillate. j. Once the liquid level reaches to within the height of the stirbar, cease the distillation by raising the remaining liquid RBF out of the oil bath, close the vacuum line, and quickly open and close the argon supply line to re-equilibrate the pressure. k. Cool if necessary and remove RBF flasks. l. Turn off the vacuum pump below the fume hood and quickly open a free vacuum line to remove vacuum in the line. m. QUICKLY remove vacuum trap dewar and place in fume hood to melt trapped liquid n. Dispose of liquid in trap and dewar, clean trap and dip pipe with appropriate low boiling point solvent (e.g. acetone), dry apparatus COMPLETELY before fastening trap and empty dewar into place, close all vacuum lines, and turn the vacuum pump back on below the fume hood. 4 Appendices Minimum safe working height of fume hood sash Fume Hood 1 Fume Hood 2 (~30cm) Vacuum Vacuum pump 1 pump 2 Appendix 1: Fume hoods containing vacuum lines in FRNY 2182. 5 Reserve tank FumeFume HoodHood 21 SupplySupply TankTank N2 purge- dry tank Appendix 2: N2/Ar compress gas cylinders for vacuum lines. Tank pressure Regulator supply indicator pressure (bar/psi) Tank open/ close valve Regulator supply Supply pressure on/off needle adjustment valve valve (bar/psi) Appendix 3: N2/Ar regulator for vacuum lines. 6 Schlenck Line Vacuum supply line pressure (torr) Inert gas supply Vacuum line to line regulator vacuum pump (L/min) Vacuum supply valves (along top Liquid nitrogen to each port) vacuum trap Inert gas supply valves (along bottom to each Vacuum supply port) line (to each port) Vacuum/inert gas port s (to reaction Inert gas supply vessel) line (to each port) Bubbler Appendix 4: Vacuum line setup.
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