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1.

Process
This SOP outlines many of the necessary precautions important for “Safe operation of a glove
box”: Last Revision: May, 2013.

2. Hazardous Chemicals Involved


Argon is used in the glove box. Although inert, it poses a risk of asphyxiation by displacing
oxygen. Hydrogen (5% in argon) is used to regenerate the purifiers. There is a low risk of flammability
from this gas. Therefore, compressed gas cylinders should always be handled in the manner outlined in
this SOP. Activated carbon is used to trap solvent. It poses an inhalation hazard.

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.

6. Special Handling Procedures and Storage Requirements


In Case of Accidental Oxygen Introduction (>50 ppm)
1) Turn off purifier circulation.
2) Open solvent trap by-pass, then close solvent trap. Order is important to not stress the blower.
3) Open the purge valve. Purge to less than 50 ppm. Close the purge valve.
4) Open solvent trap, then close by-pass.
5) Turn purifier circulation back on.

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.

9. Spill and Accident Procedures


In the event of a solvent spill in the glove box, absorbent material should be used to soak up the
liquid. It should then be immediately removed from the glove box and disposed in a proper hazardous
waste bag. As with all our labs, a lab coat and nitrile gloves are required when handling solvents outside
the glove box. Report all accidents and spills to the safety contacts: Dr. Daniel Hallinan and Onyekachi
Oparaji.

10. Waste Disposal


Any chemically contaminated material generated in the glove box should be removed, labeled
as hazardous waste, and placed in the hazardous waste collection area.

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.

12. Process Steps


To Use an Antechamber
Check that the antechamber is at atmospheric pressure.
Confirm that refill is closed/off.
Manually confirm that the other antechamber door is closed. If others are working in the glove box at
the same time, check with before proceeding.
Open the outer door.
Place sample inside.
Repeat the following procedure three times:
1) Evacuate. Allow the pressure gauge to stop moving. Continue evacuation for an addition 30
seconds for a small antechamber or 5 minutes for a large antechamber.
2) Refill the antechamber to, at least, halfway full. Do not refill the antechamber completely,
except on the third refill. On the third refill continue refilling for 10 seconds after reaching
atmospheric pressure to ensure equilibration with the glove box pressure.
Note: Antechambers are refilled with the glove box gas. If the chamber is not refilling,
something may be blocking the port. When refilling the large antechamber, the glove box
pressure will decrease to the lower working limit. At this point, refill will be paused while
the glove box is filled from the argon tank.

* 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.

To Change the Working Limits


Touch the box that shows the pressure and water and oxygen levels.
To adjust a working limit, touch the number. A key pad will appear. Type in the new number desired.
Press the “Okay” button. The change will not be executed until exiting, by pressing the “End” button.

*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.

Settings when not in use


Upper working limit > 5 mbar
Lower working limit > 2 mbar
All antechambers under evacuation
Compressed argon cylinders have sufficient pressure (>500 psi) to allow for periodic refill of the glove
box.
Purifier circulation is ON
Box light is OFF
Glove box gloves are always tied off inside the glove box.
Any known problems with the glove box that will compromise dry, inert environment have been
corrected.
*Do not pull gloves all the way out of the glove box and leave them there. They can easily become
punctured or cut and the glove box purity can become compromised and the gloves have to be switched
out.

Settings during use


These will vary with procedures being performed, but general guidelines follow.

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.

Compressed argon cylinder exchange


If the pressure becomes low in the compressed argon tank, a new tank must be attached to the glove
box supply. The procedure for doing so follows.

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).

Regeneration (specialized training required)


*Antechambers that use the same vacuum pump as regeneration should not be evacuating when
regenerating. In addition, regeneration should not be performed while the glove box is being used.
Typically, regeneration is performed overnight.
*Do not regenerate when the oxygen concentration is high in the glove box. This is because the purifier
is refilled from the glove box. In this case, purge to less than 50 ppm before beginning regeneration.
In glove boxes with two purifiers, one can be regenerate while the other is running.

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.

Solvent trap carbon exchange (specialized training required)


The carbon should be changed every six months.
Wear a lab coat, nitrile gloves, and dust mask.
1) Isolate the solvent trap from the glove box.
2) Drain the carbon from the bottom into a hazardous waste bag for disposal.
3) Cap the bottom fitting. Refill using the top fitting and a disposable paper funnel. The solvent trap
requires a little less than 5 kg of carbon pellets.
4) Evacuate for 48 hours.
5) Refill to atmospheric pressure.
6) Reconnect solvent trap to glove box.
7) Sign and date “Solvent trap carbon exchange completion log”.

Changing Gloves (specialized training required)


Once per year or when a hole
Seal glove port from the inside using another glove.
Turn off circulation; pump up the glove box pressure and working pressure limits.
Take off the old glove.
Thoroughly clean and dry a new glove.
Starting at the finger tips, roll it with knuckles aligned vertically and the thumb on top.
Stuff the rolled glove in the port.
Fold the open end of the glove over the white port.
Replace O-rings that hold the glove in place.
Remove the port seal and purge the glove box.
Sign and date “Glove change” sheet.

Changing HEPA Filters (specialized training required)


Change once per year.
Place the new filters in an antechamber. Evacuate the antechamber overnight.
If the oxygen increases when bringing the filters into the glove box, return them to the antechamber and
evacuate further.
Unscrew the old filter. Screw in the new filter.
Dispose of the old filter.

Vacuum Pumps (specialized training required)


Change the pump oil every six months. This should be done more frequently when the box gets heavy
use.

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”.

Water Sensor Cleaning (specialized training required)


Circulation off
Pressure up
Sensor out
KF 40 cap
Unscrew cover
Rinse with DI water
Air dry 10 minutes
Spread a light coat of phosphoric acid with Q-tip.
Air dry completely
Replace sensor
Purge for 10 minutes (to get real reading in box, Quick purge gives this)
Sign and date “Water sensor cleaning completion log”.
Signatures
Name Signature Date

By signing this document, I am stating that I am familiar with the hazards described in this procedure.

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