Glove Box Standard Operating Procedure

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Standard good practice

  • Remove all sharp jewelry that can catch on the gloves; using a pair of lab gloves or the cotton gloves provided in HH323 will also help with this.
  • Be conscious of what you are bringing into the box; whether that is being careful with sharp objects inside the box (and removing them when you are done) or making sure your vials are uncapped and heated before transfer, etc.
  • Use solvents only in the wet (4-glove) box; the 2-glove box should be reserved for characterization.
  • Make sure to unscrew the large “T” chamber door (inside glovebox) all the way before opening it; the o-ring can become damaged if the door is not completely unscrewed.
  • When in doubt, do the 3 evacuation/refill steps before you open a transfer chamber to the box.
  • Let someone of authority (i.e. Ingrid Anderson, Jim Johnson, or Joe Beach) know if you encountered a problem with contamination while using the box. These sorts of things happen(!); it’s just good to keep track of them.

Using the small antechamber to transfer in/out of the glovebox

Transferring materials into the glovebox

  1. Inspect the setting of the toggle switch on the small antechamber; it will either be pointing toward ‘vac’, ‘gas’ or neither (the pressure gauge should read ~ -25inHg, 0inHg, or other, respectively).
  2. Prepare the chamber for exposure to atmosphere. If vacuum is being pulled, point the toggle to gas until the pressure is at equilibrium with atmosphere, if the toggle is pointing toward ‘gas’, make sure it goes to the neutral center position to avoid contamination of the box, while if the gauge is reading some intermediate pressure between 0 and -25 inHg, evacuate and backfill the chamber.
  3. Check that the toggle is in its neutral center position. Open the small outer door by lifting up on the red lever. Place your materials into the chamber and close the door.
  4. Perform three evacuate/refill cycles before moving items into the glovebox box by moving the toggle on the antechamber from the ‘vac’ setting to the ‘gas’ setting three times. The length of the vacuum cycle will depend on what you are transferring to the box. Large equipment, kimwipes, paper, etc. require a much longer time in the transfer chamber so that adsorbed water can be removed (e.g. all of these items must be pumped on for 24 hours minimum). The length of the vacuum cycle just requires some common sense. If you are moving glassware in and out, for example, make sure it has been heated before the transfer so that a minimum of water will get in; make sure to uncap vials, etc. For small items that pose no risk of contamination, the small antechamber requires a vacuum purge of a minute or two, until the reading on the pressure gauge is at -25 inHg or so. You must backfill with box atmosphere until the pressure comes up to 0 inHg.
  5. Place the toggle to the neutral center position, and move your materials into the glovebox.

Transferring materials out of the glovebox

Perform 3 evacuate/refill cycle before opening the chamber up to the box, regardless of whether there is anything in the transfer chamber or not. (See the Transferring materials into the glovebox section above for details of how to perform the evacuate/refill cycles.) Note: if you are transferring something into the glovebox and are subsequently pulling something out, you do not need to re-complete the evacuate/refill cycles, as long as the transfer chamber has not been opened to atmosphere during your time using it. If you leave the chamber unattended, or are unsure of whether the chamber is filled with box atmosphere or air, you must complete the evacuate/refill cycles before transferring something out of the box. When it doubt – just do the evacuate/refill cycles.

Using the large “T” antechamber to transfer in/out of the glovebox

Transferring materials into the glovebox

  1. Inspect the setting of the green pushbuttons near the large antechamber; either ‘EVAC or ‘REFILL’ or neither will be illuminated (the pressure gauge should read ~ -25inHg, 0inHg, or other, respectively).
  2. Prepare the chamber for exposure to atmosphere. If vacuum is being pulled, push the ‘REFILL’ button until the pressure is at equilibrium with atmosphere; if the toggle is pointing toward ‘REFILL’, push the ‘REFILL’ button again to avoid contamination of the box; if the gauge is reading some intermediate pressure between 0 and -25 inHg, evacuate and backfill the chamber, taking care to re-push the ‘REFILL’ button (so that the light goes off) when done.
  3. Check that neither of the buttons are illuminated. Open the large outer “T” door by rotating the handle. Place your materials into the chamber and close the outer chamber door.
  4. Perform three evacuate/refill cycles before moving items into the glovebox box by pushing first the green ‘EVAC’ button. The length of the vacuum cycle will depend on what you are transferring to the box. Large equipment, kimwipes, paper, etc. require a much longer time in the transfer chamber so that adsorbed water can be removed (e.g. all of these items must be pumped on for 24 hours minimum). The length of the vacuum cycle just requires some common sense. If you are moving glassware in and out, for example, make sure it has been heated before the transfer so that a minimum of water will get in; make sure to uncap vials, etc. For small items that pose no risk of contamination, the large “T” chamber requires a minimum vacuum evacuate time of at least 5 minutes. This means the total minimum time for a transfer in the large transfer chamber is 15 minutes. Backfill with gas by pushing the green ‘REFILL’ button and waiting until the chamber is half pressurized, that is until you are reading around -12inHg on the pressure gauge. Return to the evacuation step (again, this process must occur 3 times).
  5. Push the ‘REFILL’ button again (so that none of the green buttons are lit), and move your materials into the glovebox by rotating the handle inside the glovebox. Note: You must unscrew the handle all the way, or the o-ring on the door could become damaged.

Transferring materials out of the glovebox

Perform 3 evacuate/refill cycle before opening the chamber up to the box, regardless of whether there is anything in the transfer chamber or not. (See the Transferring materials into the glovebox section above for details of how to perform the evacuate/refill cycles.) Note: if you are transferring something into the glovebox and are subsequently pulling something out, you do not need to re-complete the evacuate/refill cycles, as long as the transfer chamber has not been opened to atmosphere during your time using it. If you leave the chamber unattended, or are unsure of whether the chamber is filled with box atmosphere or air, you must complete the evacuate/refill cycles before transferring something out of the box. When it doubt – just do the evacuate/refill cycles.

Oxygen or water contamination

The box is set up with isolation valving so that if, for example, box 1 gets contaminated, flow will be interrupted to box 1 and box 2 will continue to receive uncontaminated atmosphere. If the oxygen values get above 200ppm, the isolation valving will be tripped (this makes an audible sound), and the screen will show that contamination has occurred. In the case that this happens to you, follow the subsequent steps for restabilizing the box you are working in. It is important to realize, however, that unless you have isolated the cause of the contamination, this set of steps will not really help much, so it is best to figure that out before you go through the rest of this:

Purge the box

  1. From normal operation mode on screen, verify that circulation is off. If circulation is still on, press F5 to turn it off.
  2. Switch active box to box with the alarm condition:
    1. Go to the service mode by pressing Esc from normal mode or F3 from main menu
    2. Press Enter twice to go through the User menu to the Service mode
    3. Arrow down to get to Box selection
    4. Set the active box to the box with contamination by using arrow/enter keys
    5. Press Esc twice to return to the main menu
  3. From the main menu press F6 to start the automatic purge. This should be set to 20 minutes. To increase the purge time:
    1. Go to the service mode by pressing Esc
    2. When User menu is shown, press Enter
    3. When Service menu is shown, press Enter
    4. Arrow down until you reach the purge time menu; press Enter
    5. Enter password (2905) by using the arrow and enter keys
    6. Adjust set point by using arrow keys; press enter
    7. Press Esc twice to return to the main menu
  4. After purging is complete (or to check oxygen levels at any time) press F1 to return to normal (circulation) mode.
  5. If oxygen/water levels are still too high, the box will shut off again. You can either choose to purge for more time (this is better for the gas reactor but will use more nitrogen) or turn off the isolation valving until the reactor has purified the air. To turn off the isolation valving:
    1. Go to the service mode by pressing Esc
    2. When the user menu is shown, press Enter
    3. When the service menu is shown, press Enter
    4. Arrow down until you reach the Set Analyzer Alarm delays selection
    5. Set the Alarm delay to zero with the arrow/enter keys; this will disable the isolation valving
    6. Press Esc twice to return to the main menu
  6. If oxygen levels have returned to low levels, reactivate the box isolation system by setting a non-zero delay time for the alarm system (see step 5), and reset Autopurge time to 20 minutes if you have changed this value (see step 3).
  7. Please let Ingrid Anderson (ianderso@mines.edu) or Joe Beach (jbeach@mines.edu) know there was contamination that shut down one of the boxes; it will factor in to when the next regeneration happens.

Using the solvent purification system

Inside the glovebox

Turn the tap on and put an appropriate storage container underneath the tap. It is important to cap your storage container so that the box atmosphere does not get too full of solvent vapors. There is a solvent trap but it has limited capacity.

Outside the glovebox

The solvent collection method you use outside the glovebox will not affect atmosphere in the box, however, it is a waste of the solvent purification system to use solvents that will subsequently be used in atmosphere. It is recommended that you perform 3 evacuate/refill cycles of your solvent storage container (similar in principle to what one would do for transfer in and out of the glovebox) in the manner described below:

  1. Turn on vacuum pump and inert gas supply; make sure all solvents’ toggles are set to the closed position
  2. Put collection vessel on the jack stand in the cork ring, and attach to spout. The system is currently configured for a round bottom flask with a side syringe port and 24/40 neck. These instructions will assume you have a valve on both the neck and side port.
  3. Turn lower toggle to ‘Vac/Gas’ setting.
  4. Perform three evacuate/refill cycles: close side port valve and open neck valve; set upper toggle to ‘Vacuum.’ Let pressure come down to about 28inHg, as seen on pressure valve. After you have achieved this or whatever pressure you want, toggle to ‘Gas’ for one second. Repeat evacuate/refill twice more.
  5. Evacuate vial one more time by toggling to ‘Vacuum.’
  6. Turn upper toggle to ‘Closed.’
  7. Turn lower toggle to ‘Dispense’ to collect solvent.
  8. Turn lower toggle to ‘Vac/gas.’
  9. Turn upper toggle to ‘Gas’ for a few seconds to pressurize flask.
  10. Turn upper and lower toggles to ‘Closed.’
  11. Close neck valve and remove flask by adjusting jack.
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