Glove Box Operating Procedure

Some Common rule of thumb:

Glovebox is an isolation device, Never Open It to Air. (e.g. open both doors of the same antechamber, move things into the box without pumping).

No sharps near the gloves, minimize the use of sharps inside the box and use extreme caution when you have to.

The antechambers should be under dynamic vacuum (i.e. vacuum switch should be in the ‘on’ position while not in active transfer).

Minimize solvent evaporation inside the glovebox.

-Normal range of glovebox parameters on the LCD display: pressure ( ~ 2-6 mbar) moisture level ( < 0.1 ppm)and freezer temperature (< -10 °C), usually -19). Circulation on (the CKM icon should be purple instead of grayed out).

-Alarm BZ if any of the parameters is out of range.

Moving materials into glove box.

-Check logbook for the antechambers to ensure that nothing is being kept under vacuum presently.

-If antechamber is free than check vacuum gauge to ensure antechamber is under a stable vacuum (-28 to -30 in Hg).

  • IF VACUUM GAUGE READS -25 in Hg TELL BZ.

-Document which antechamber, operator, material, and time as detailed in the log-book.Date the entry if you are the first user of the day.

-Fillantechamber with N2until vacuum gauge reads 0 in Hg. (This can be done relatively quickly)

-Place you material into antechamber. (This should be contained within a secondary plastic container whenever possible).

-Cycle vacuum/N23x. Depending on what is being moved into glove box, differing levels of conservation when evacuating and refilling chamber should be used.

  • Powder = gently evacuate and refill the chamber to avoid losing fine or fluffy powders
  • Liquid, if packed under vacuum, can be moved in as is. If packed under N2, then double septum and reinforce with copper wire. If packed under air, run freeze/pump/thaw cycle before placing it in the chamber.
  • Glassware/metal spatula = fast evacuation and refill can be used
  • Porous materials (weigh paper, kim wipes, cork ring etc.) should be evacuated for extended periods of time (overnight to days in the big antechamber).

-Once material has been cycled appropriately, fill antechamber with N2 (until vacuum gauge reads 0 in Hg) then isolate antechambers from glovebox (close position for the small chamber).

  • The pictures below depict what the valves look for each antechamber when they are isolated from glove box.
  • A. is the small antechamber
  • B. is the larger antechamber
  • The yellow valve is for N2 flow
  • The black valve (circle) is for vacuum.

Moving materials out of the glove box.

If the antechamber is under vacuum,

back fill with N2,

open the inside door,

place materials in the tray,

closethe inside door,

open the outside door,

move materials out,

close the outside door and pumpdown the chamber.

If you just moved things in and the chamber is under N2, you can move things right out without pump/backfill. If your operation inside the box is longer than 10 min, pump it down.

Operating inside the Glove Box

-On the touch screen check the display for pressure ( ~ 2-6 mbar) and moisture level ( < 0.1 ppm)

  • IF EITHER OF THESE READINGS DOES NOT MEET THESE VALUES TELL BZ.

-Change the lower working limit to - 0.5 mbar

  • Hit end or back to return to original screen.

-Place cloth gloves on and put hands into black plastic gloves.

  • Do this in a controlled, slow manner as not to raise the pressure too fast
  • Or lower pressure inside of glove box using left foot pedal before entering glove box.

-Now you can move your materials from the antechamber into the glove box.

After removing material from either antechamber make sure to close antechamber door to minimize any leaks. If your operation inside the box is longer than 10 min, pump the chamber down.

-Post-operation procedure:

-Remove materials and all trash accumulated into secondary plastic container and inside of appropriate antechamber.

  • Ensure glove box is clean before finishing work.

-Close inside antechamber door.

-Remove materials/debris/trash from antechamber and close outside antechamber door.

-Evacuate antechamber and leave it under vacuum.

  • Make sure reading on vacuum gauge is stable and below -28 in Hg, which indicates that antechamber doors have been closed properly.
  • If vacuum gauge can NOT reach below -28 in Hg, there is a leak at one of the chamber doors and should be fixed immediately.

-Go back to touch screen and change lower working pressure limit to 2 mbar.

-Once completely finished make sure of the following:

  • Touch Screen displays:
  • Pressure reading = 2-6 mbar
  • Water reading = < 0.1 ppm
  • Freezer temp <-10°C
  • Vacuum gauges on antechambers read -28to -30 in Hg
  • Circulation and vacuum pump are on

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