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This SOP outlines many of the necessary precautions important for “Safe operation of a glove
box”: Last Revision: May, 2013.
3. Potential Hazards
Air sensitive materials, such as lithium, are used in the glove box. Therefore, protocols outlined
in this SOP are important to maintain low levels of oxygen and water. Refer to the SOP on “Lithium
Handling” for details of proper lithium handling.
4. Approvals Required
All researchers will be trained in proper glove box procedures. Researchers will not be permitted
to use the glove box until they have been trained as well as read and signed this SOP. General EH&S
training is required to access and use the labs.
5. Designated Area
Glove boxes are located at the AME building room 232.
Troubleshooting
If purging stops, it is probably because the line pressure has dropped below 55 psi. This can be avoided
by increasing pressure at tank regulator. If the tank runs out of gas, purging must be stopped and the
tank replaced. The tank regulator should be operated at 80 psi. The steady-state pressure of the box
during purging can be adjusted by controlling the position of the purge valve.
7. Personal Protective Equipment (PPE)
Safety glasses are to be worn at all times. Cotton or uncontaminated nitrile gloves may be worn
between the hands and the butyl glove box gloves. Nitrile gloves should be worn inside the glove box
(over the glove box gloves). A lab coat is recommended. Arm sleeves may also be worn.
8. Engineering/Ventilation Controls
The exhaust of the vacuum pumps, regeneration gas, and glove box vent to the building
ventilation system. Note that the glove box only exhausts during purging.
11. Decontamination
It is important to maintain a clean environment, especially in glove boxes where battery
assembly occurs because of the sensitivity to contamination. Before commencing work in the glove box,
aluminum foil should be used to cover the work surface. After completing work, all trash should be
collected in the foil and removed from the glove box. In addition, any common supplies, such as
tweezers, hot press, cutting board, micrometer, should be wiped clean of any contamination such as
polymer or powder. Under no circumstancing may a new material be introduced to the glove box
without prior approval by the PI. In particular, this includes halogenated solvents which will destroy the
purifier and electrochemically active material that is volatile.
* For small antechambers, always place the hand valve in the closed position before opening the
antechamber door. For large antechambers, always turn off refill before opening the antechamber door.
* The handle on the small antechamber only needs to be finger tight. Turn the large antechamber
handle until it stops. Do not over tighten the antechamber handles.
* Never open more than one antechamber door at a time.
* Always perform the above procedure before opening the inner antechamber door, even if you have
not opened the outer door.
* Do not attempt to open an antechamber door when the antechamber is evacuated. This can deform
the door and compromise the seal.
*Do not change the working limits while refilling an antechamber. All pressure regulation is suspended
while in the working limit set screen. Entering this screen while refilling an antechamber can cause the
glove box to become severely under-pressurized.
*After selecting new working limits review them and make sure the selected numbers are the actual
numbers meant to be typed in before hitting the end button. Selecting pressure levels too high can
result in deformation of plexiglass and may result in the plexiglass being blown out.
If a box becomes over-pressurized (>15 mbar), it will disable the sensors and purifier circulation.
The pressure should decrease to within the working limits automatically. If it does not, do so manually
using the left pedal. The working limits (typically 0 mbar lower and 10 mbar upper) can be checked and
adjusted by touching the actual pressure reading on the main screen. After the pressure is within the
working limits, re-enable the sensors and purifier circulation by pressing the functions button on the
main screen. Next press the “Analyzer” and “Circulation Purifier” buttons so that they become green.
If the oxygen or water content in the box becomes >100 ppm, then “Quick Purge” can be used.
This option is available on the functions screen when purifier circulation is off.
Please do not perform more complex operations, such as purifier regeneration, without first
being trained by an experienced user.
The manuals are available in the manuals cabinet of AME 232.
1) Close valves to glove box, beginning with the valve closest to the box.
2) Close empty (or nearly empty) cylinder.
3) Purge tubing between empty cylinder and first (closed) valve to glove box.
4) Disconnect and cap empty cylinder.
5) Uncap and connect new cylinder. Confirm that cylinder contains correct gas. Note that
regeneration gas is reverse threaded.
6) Open new cylinder.
7) Check for leaks from fittings using soap water.
8) Purge tubing between new cylinder and first valve to glove box.
9) Open valves to glove box, ending with the valve closest to the box.
10) Sign and date “Compressed argon cylinder exchange completion log”.
Note: The regulator inlet from the cylinder should read approximately 2500 psi. For a manifold set-
up such as 70-123 and 62-348, the regulator nearest the cylinder should have an outlet pressure of
about 150 psi (should not need to be adjusted). The outlet pressure to the glove box should be 80
psi (also should not be adjusted).
1) Confirm that the regeneration gas is connected correctly and contains at least 700 psi. Also check that
the argon tank contains at least 500 psi.
2) In the functions menu press the “Purifier Regen” button.
3) Confirm that you want to regenerate by pressing the button that appears in the middle of the screen.
4) Using the valves leading to the glove box, adjust the flow rate from the 5% hydrogen in argon tank so
that the flow meter reads 15-20 L/min. You may need to first run a high flow rate to blow condensed
water out of the flow meter in order to get a stable flow rate.
4) Confirm gas flow by pressing the flashing button/message.
At this point the regeneration procedure is on auto pilot. It takes about 12 hours to complete.
1) Heats filter column.
2) Purge special gas: 95% argon 5% hydrogen at 4 psi
3) Evacuation cycles
4) Finishes/stops automatically.
The next day, check the pressure decrease of the regeneration gas. It should lose 700-800 psi. Close the
valves and tank.
Check the regeneration effluent. It should contain 40-50 mL of water. This is often not the case because
it evaporates in the regeneration flow. However, if the effluent has any chemical smell, the solvent trap
carbon must be replaced immediately.
1) Set the upper working limit to 14 mbar so that the glove box will not call for vacuum during this
procedure, which would expose it to atmosphere.
2) Turn off purifier circulation. Turn of the vacuum pump on the screen and at the pump. Unplug the
pump.
3) Disconnect the pipe to the vacuum pump. Cover the pipe with a blank KF fitting.
4) Take the pump off the tray.
5) Remove the plug and pour out the oil. Loosen a fitting on top for easy pouring.
6) Replace the plug and refill the oil to almost the maximum fill line.
7) Change mist filter once per year. It can clog and affect the pump as well as spilling oil.
8) There is a black hose that recycles oil from the mist filter back to the pump. It contains a flow
restrictor that can get clogged. Acetone will easily clear such a clog.
9) Sign and date “Vacuum pump oil exchange completion log”.
By signing this document, I am stating that I am familiar with the hazards described in this procedure.