Equipment Operating Procedure Glove Box

Transcription

1 Equipment Operating Procedure Glove Box Page 1

2 0.0 Changing the Compressed Gas Cylinder 1. Complete Compressed Gas Cylinder training from EHS website before manually exchanging gas cylinders. In order to access gas cylinders stored in Scott Lab, request the garage key from the 3 rd floor office. Scott Lab office keys have access to cylinder storage. Cylinder storage is the 2 nd door on the left in the 1 st floor garage in West side of Scott Lab. 2. To remove current cylinder, turn valve on top of tank clockwise to close it. 3. Using a wrench, twist the bolt connecting cylinder to safety valve in an upward motion to loosen it. Continue twisting the bolt until the safety valve is removed. Replace protective valve covering on gas cylinder. 4. Important: Tear off the contents tag on the cylinder to show the tank is Empty. 5. To attach new gas cylinder, remove protective valve covering and insert the safety valve in the port on top of the cylinder. 6. Using a wrench, screw the valve bolt in a downward motion to tighten it completely. 7. Turn the control valve in top of the cylinder counter-clockwise to open flow from cylinder. 8. Tear off the contents tag on the cylinder to show the tank is In Use. 9. The cylinder is now fully attached and ready to use. 1.0 Antechamber Controls These steps assume the atmosphere in the glove box is purified and not open to the outside air. Security Code for glove box controls: Large Antechamber Inserting an Item into the Glovebox 1. Important: Verify the antechamber contains purified gas before opening the inner door. 2. Ensure the inner door and refill valve are fully closed. 3. Open the outside door and insert the object into the Antechamber. 4. Close the outside door and open the vacuum valve and evacuate to -29 in. Hg. 5. Close the vacuum valve and open the refill valve until pressure reaches -15 in. Hg. 6. Repeat evacuation and refill at least 3 times, finally reaching atmospheric pressure. 7. Close the refill valve and open the inner door to remove the object from the chamber. Page 2

3 1.1.2 Removing an Item from the Glovebox 1. Ensure that the outside door and refill valve are fully closed. 2. Open the inner door. 3. Insert the object into the Antechamber and close the inner door. 4. Open the outside door and remove the object. 5. Purge the antechamber before re-opening the inside door. 1.2 Small Antechamber Inserting an Item into the Glovebox 1. Ensure the inner door and 3-way valve for mini-chamber are fully closed. 2. Open the outside door and insert the object into the Antechamber. 3. Close the outside door and turn 3-way valve to evacuate and evacuate to -29 in. Hg. 4. Turn the 3-way valve to refill until pressure reaches -15 in. Hg. 5. Repeat evacuation and refill at least 3 times. 6. Close the 3-way valve and open the inner door to remove the object from the chamber Removing an Item from the Glovebox 1. Important: Verify the antechamber contains purified gas before opening the inner door. 2. Ensure that the outside door and 3-way valve are fully closed. 3. Open the inner door and insert the object. 4. Close the inner door. 5. Open the outer door and remove the object. 6. Purge the antechamber before re-opening the inside door. 2.0 Removing Front Panel to Expose Glove Box 1. Verify that toxic materials will not be present inside of glove box at the time. 2. If planning to purge glove box and reset inert Argon atmosphere, verify that at least six (6) full tanks of argon are available for the glove box. 3. Close valve on argon tank by turning the valve clockwise. Page 3

4 4. Turn off power to glove box my pressing switch on front-facing panel located beneath antechamber. 5. Raise light fixtures over the top of the glove box. Light fixtures rotate along hinge. 6. Remove gloves from the front panel by removing the two bands securing the glove and then pulling off the glove itself. 7. While carefully holding onto the front panel, open each safety lock sealing the front panel and the glove box. IMPORTANT: Start at the top, work down the sides, and finally unlock the bottom. 8. Warning: Avoid letting the panel edge contact the sealing on front of glove box. This may lead to a scratch that prevents the seal from forming when system restarts. Be extra careful when removing the front panel from the glove box. Set the panel aside. 3.0 Restarting Glove Box after Exposing Atmosphere 1. Make sure at least 6 full argon tanks are on hand to purge and refill the glove box. 2. Verify that all seals are secured on front panels, each antechamber door is tightly closed, exhaust system is functioning, and cooling system is functioning (if applicable). 3. Note: If a front panel was removed from the glove box at any point, clean the seal with rubbing alcohol and apply high vacuum grease. 4. Turn on argon feed to the glove box by turning the top valve clockwise. 5. Turn on glove box power using the switch located on the front panel beneath the antechambers. 6. Perform a pressure check on the glove box (see section 5.0) 7. (step 5-8 is the purging method for the antechamber) Set the Working Maximum pressure to mbar and the Working Minimum Pressure to +5.0 mbar. To do this, press the System Config. button and adjust the numeric values with the blue display. The working gas will enter the box automatically. 8. Turn on the vacuum pump by pressing the Start button on the main screen. 9. Open the evacuate valve on the Large Antechamber and allow the chamber to evacuate to evacuate to Close the evacuate valve and repeat for the mini antechamber. 11. Wait 10 minutes for the glovebox to stabilize. 12. Use the appropriate foot pedal to add/remove gas to/from the glovebox to reach desired pressure. 13. Important: See section 5.0 to perform a pressure test on the glove box and verify that all seals are secured. 14. It is extremely important to purge the glove box to displace as much air in the box as possible with inert gas. Important: Purging the glovebox requires 3 full cylinders of Page 4

5 working gas (6 cylinders for large glove box). Follow the steps in section 4.0 to purge the system. 4.0 Purging the Glovebox 1. Purging the glove box requires 3 full cylinders of working gas (6 cylinders for large glove box). Verify sufficient cylinders are in inventory (lab and 1 st floor garage). 2. Set Working Maximum pressure to mbar and the Working Minimum Pressure to +5.0 mbar (see section 3.0). 3. Open the manual purge valve located on the back panel of the glove box beneath the antechambers. 4. Adjust the flow using the purge valve so that there is a steady flow of incoming gas and the box pressure is maintained at >1 mbar. 5. Create turbulence in the box to increase purge efficiency. This can be done by pressing in the gloves or using an electric fan or vacuum inside the glove box. 6. As the working gas cylinder empties, close the purge valve and change the cylinder. Open the valve on the cylinder and then re-open the purge valve. 7. Purge the system with the required number of cylinders or until Oxygen content is 25 ppm or less. Then close the manual purge valve. 8. The oxygen content might increase once the blower has been turned on (Main Screen -> Blower Control). If oxygen level rises above 100 ppm, stop the blower and continue to purge. 9. The blower system circulates the atmosphere through the purification system. It can be set to low speed during weighing, or set to high speed to recover from operator error. 10. Set the blower to 50% during normal operation. (100% = full blower speed) 5.0 Preforming a Pressure Test (Check Seal Quality) 1. Perform a pressure test anytime the front panel of the glove box is removed and replaced. A pressure test should also be performed periodically for safety and quality assurance. 2. Close purge valve located on back of glove box panel beneath antechamber. 3. Turn compressed cylinder on by rotating the valve on top of the cylinder counterclockwise. 4. Set Maximum Working pressure to 12.0 mbar and the Minimum Working pressure to 10.0 mbar. Page 5

6 5. Allow 10 minutes for the glovebox to stabilize at 11.0 mbar. Use the foot pedals to finely adjust the pressure. 6. Watch the current pressure in the glove box carefully for 25 minutes. If the pressure fluctuates more than 1 mbar, the system is not secured. Troubleshoot the seals/connections or contact Innovative Technology Inc. 6.0 Regenerating Purification Columns (Single-Column, offline) 1. Make sure that regen gas tank is sufficiently full. Column regeneration consumes approx. one-half of the tank. 2. Unless a second purification column is installed, the atmosphere of the glove box will be jeopardized so all experiments should be stopped and all chemical containers should be closed tightly. 3. Connect a cylinder of regenerating gas (3-7% Hydrogen in Nitrogen or Argon) to the regen gas connections (cylinder in left position if looking at them). Ensure connections are tightly secured. 4. Open the valve on top of the tank, allow the gas line to fill. Set the regulator pressure to 7 psi. 5. Turn off the blower on the main screen. 6. Press the Start button in the Regen Controls menu. The screen will prompt the user with two questions. 7. Are the column valves closed? Make sure that column valves are closed. These are located on top of the purification column inside the purification box. If the yellow valves are visible, the column valves are not closed. 8. Click Yes in the blue box next to the question. A click will be heard; the solenoid valves are opening to allow regen gas to flow. 9. Is Flow OK? At this point, the regen gas should have built up pressure and is ready to flow through the purification chamber. Adjust the needle valve on the front of the purification box to set the flow between scfh. The flow indicator should be held steady in between these two value. 10. Click Yes in the blue box next to the question. Now the regen gas will stop flowing and the flow indicator will drop to 0. The flow will automatically restart after the column is sufficiently heated (default = 3 hours). 11. The remainder of the column regeneration is automatically controlled by the glove box. The default time is 14.5 hours. At the end of the cycle, the blower will automatically turn back on. Page 6