Glove box Keep log of Oxygen and Moisture levels to track the operation of the glove box components. Keep ports under vacuum so they are always oxygen and moisture-free. To bring materials out: refill with nitrogen, open the inner port door, put materials into port, close inner port door, open outer port door, remove materials, close outer port door, pump down again with vacuum. Instructions for Bringing Materials into Glovebox See page 15 in User Guide Also: 1. Uncap all containers to avoid bringing moisture and oxygen in, and to avoid breaking the container. 2. Liquids: Deoxygenate first with freeze-pump-thaw cycles or argon/nitrogen bubbling and bring into box capped. 3. Solids: Remove cap from container, cover with chem wipe and rubber band. Pump and refill slowly. If your reactions require water as a solvent, make sure that the other chemicals and materials in the box are safe and not damaged by this. When running the reaction, follow these steps: 1. Close the circulation valves to protect the catalyst. 2. Turn the oxygen sensor to Air Cal. 3. Turn off the fan (press Blower Control on the control panel). 4. Run your reaction, as quickly as possible in order to minimize the amount of moisture in the box. 5. Purge the glovebox until moisture levels are a few ppm (see pp. 11 and 15 in User Guide). 6. Turn fan on, turn oxygen sensor back to Sample, Open circulation valves. See User Guide for help in finding valves and controls. Regular and Semi-Regular Maintenance See Omni-Lab System User Guide for maintenance and troubleshooting help on each topic except changing tanks and vacuum pump oil Changing the moisture probe Frequency: Calibrate every ~1 year, send back to factory Changing fuel cell (oxygen sensor) Frequency: Calibrate every ~1 month, change ~6 months to 1 year, check SPAN Catalyst regeneration Frequency: When oxygen level is suddenly much higher than usual and the fuel cell oxygen sensor is not the problem Changing nitrogen (Inert gas) and 5-7% hydrogen/nitrogen (Regeneration gas) tanks Frequency: Nitrogen- depends on how often purging is needed Hydrogen/nitrogen- depends on how often regeneration is needed Procedure: Close off Swagelok valve, close main tank valve, remove regulator, switch tanks, attach regulator to new tank, open main tank valve, purge line three times by releasing gas through Swagelok valve then return to open position, check for leaks with soapy water Changing vacuum pump oil Frequency: Depends on amount of solvents the box is exposed to, every ~4 months and after regeneration of the catalyst Procedure: See BOC Edwards Instruction Manual Replacing gloves Frequency: When one develops a hole, as evidenced by pressure changes in the box and large amounts of purge gas being used with no leaks are found in tubing or connections Gas tanks Our lab uses mostly compressed nitrogen (asphyxiation hazard), and some argon (asphyxiation hazard), oxygen (oxidizer, flammable), and hydrogen (flammable). Safety precautions that are relevant to the specific gas should be taken. Signs should be posted identifying substances and hazards of gases, for example: HYDROGEN—FLAMMABLE GAS NO SMOKING-NO—OPEN FLAMES General guidelines: Close the cylinder valve on a tank when it is not in use. When moving a cylinder: close the cylinder valve, remove the regulator, cap the tank, and use the cart for transport. Secure tanks to the wall with installed chains to prevent tipping and creation of a pressure driven rocket. Check for leaks with soapy water (for inert gases) or other methods (for toxic or flammable, see Prudent Practices) after installing new line or affixing regulators. Make sure fittings are matched, Teflon used only with the correct fittings, and the right regulator is chosen for the substance in the cylinder (threads are specifically designed separately for different gases- never force). In the case of a leak from the cylinder, move it to a hood if possible or to a well ventilated area if the gas is not toxic or hazardous. Call emergency services if needed. Cylinders containing flammable gases should be properly grounded. A cylinder should never be emptied to a pressure lower than 172 kPa (25 psi) because the residual contents may become contaminated with air if the valve is left open. Teflon tape should be used on tapered pipe thread where the seal is formed in the thread area. Teflon tape should not be used on straight thread where the seal is formed through gaskets or by other metal-to-metal contacts that are forced together when the fitting is tightened. Information which is relevant to our lab can be found in Prudent Practices in the Laboratory: Handling and Disposal of Chemicals. See pages 74, 88, 104, 121-127 for more details on topics such as Handling Leaking Gas Cylinders, Flammable Gases, Pressure Gauges, Piping, Tubing, and Fittings, Teflon Tape Applications