Glove Box Policies and Procedures Wooley Research Group Please read entirely before operating the glove box on your own. Before operating the glove box: 1. Check the log sheet to see if the glove box is already in use by another person. (Always make sure no one else is using the glove box!) 2. Check the gauge on the Argon tank and make sure that it is above 500 psi BEFORE purging! If it is getting close to 500 psi, please change the tank (if you don’t know how to, BE SURE to contact those in charge). Otherwise, there should be a spare Argon tank in room 1415 along with a cart. 3. If no one else is using the glove box, please fill out the log sheet completely. In an effort to have consistent monitoring of the glove box pressure, O2, and moisture levels, please fill out the values as you see them BEFORE purging or using the box. Note: Do not wear a lab coat while using the box and remember to remove all jewelry. Operating the glove box: 1. ALWAYS wear gloves on both sides of the rubber gloves! It is MANDATORY in order to protect the glove box gloves. 2. Before bringing items into the glove box (i.e. via the antechamber), make certain that the inner doors to both antechambers are closed! 3. If items need to be transferred in or out of the glove box, two antechambers can be used. Only use the larger antechamber if items cannot fit into the smaller antechamber. The transfer process for the smaller antechamber is quicker and requires less argon than that of the larger antechamber. a. Small antechamber1: i. The small antechamber should be under static vacuum. Refill the antechamber with argon by switching the valve to ‘Refill.’ Once the vacuum gauge reads zero, ensure that the knob is set to ‘Close’. ii. Open the outer antechamber door and place your materials inside and securely close door. iii. Evacuate the antechamber for 10-15 minutes and flip the sign that is hanging on the antechamber to “in use”. iv. Fill the antechamber with argon. v. Repeat steps iii and iv twice. Note: There are some items that need to be evacuated for a prolonged period of time (please see ‘Useful Box Materials’). 1 If placing paper items in the box, please read ‘Useful Box Materials’ first! vi. Now, the inner door of the antechamber can be opened and your equipment brought inside. (Recommended: close the inner door right after bringing in your equipment.) vii. When you are done with your work inside the glove box, open the inner door of the antechamber (make sure that an inert atmosphere has been maintained inside the antechamber!), put your equipment AND WASTE inside and close the inner door again. viii. Open the outer door, take out your items and waste, close the outer door again, and evacuate the antechamber right after doing so. Leave the antechamber under vacuum when not in use. ix. Complete the entry in the glove box log sheet and flip the sign, “not in use”. b. Large antechamber2: i. Ensure that the inner door of the glove box is closed. If still under vacuum, fill the antechamber with argon (see step iv). Place materials inside the chamber and close the outer door. ii. On the Main page of the touch screen, press ‘Auto-Evacuation’ to enter the antechamber auto-evacuation page. iii. Press ‘Start’ to initiate the evacuation/purge sequence. The sequence is already programmed and will take an hour to complete. Note: If needed, the sequence can be stopped by pressing ‘Stop’ before completion. iv. Once the auto-evacuation sequence is complete, return to the main page by pressing ‘Main’ on the touch screen. Open the refill valve by pressing the valve symbol that connects the box to the large antechamber. This will equilibrate the pressure between the box and antechamber. Wait until the vacuum gauge on the antechamber reaches zero. Close the refill valve. It is of crucial IMPORTANCE that this is not forgotten. v. Open the inner door and transfer materials into the box. Put anything to be removed onto the sliding tray. vi. Close the inner antechamber door. Open the outside door and remove the contents inside. IMPORTANT: Make sure that the refill valve is closed. When the refill valve and the outside door are both open simultaneously, the box is connected to the outside atmosphere. vii. Close the outer door and evacuate the antechamber by pressing the evacuation valve (one that connects the antechamber to the pump) on the Main page. This will keep the antechamber under vacuum when not in use. Note: When removing items from the glove box, never assume that the previous user has performed the necessary auto-evacuation procedure. Always perform the auto-evacuation procedure to ensure that the box is not contaminated by outside air. 2 If placing paper items in the box, please read ‘Useful Box Materials’ first! Working inside the glove box: 1. Please make sure that you have outer protective gloves on. This will prolong the life of the gloves. 2. Make sure that when using sharps that you place them at a safe distance so no accidental puncturing of the gloves occur and that they are covered with a septum. Box Solvents and Reagents 1. All solvents should be dried and degassed. 2. Try to avoid the use of volatile protic reagents such as alcohols, phenols, and amines (which react with water sensitive complexes), as well as halocarbons, and phosphines. 3. No mercury is allowed inside the glove box, since if it is spilled it will amalgamate the metal on the bottom of the glove box. Please note: Other reagents in addition to those mentioned can be damaging to the catalyst. Therefore, please keep solvent and other reagent vessels tightly closed, and minimize the amount of time they are open in the glove box. Useful Box Materials 1. The people in charge of the glove box will try to maintain a common supply of vials, pipettes, gloves, kim wipes, etc. (Please inform us if there are any other bulk items desired.) If you exhaust one of the bulk items, please notify the person in charge of replacing items. It will take at least 24 hours to replace a bulk item. 2. Paper MUST be dried in a vacuum oven overnight at 60 °C and evacuated overnight BEFORE glove box entry! 3. Glassware and other items such as spatulas should be dried and degassed. 4. Weighing boats can enter the box by a normal pump down procedure and does not require drying. Storage of chemicals: 1. All containers and vessels containing chemicals must be clearly labeled and placed in their appropriate place (i.e. no random storage of materials on the floor of the box!). Please log your chemical in the glove box inventory log book. When done with the glove box: Please check the argon pressure to see if it is still above 500 psi. Make sure that all of the waste is disposed of and that everything is clean! 1. Turn off the light (on touch screen). I, ____________, have acknowledged that I have read through the glove box operating procedures and policies and understand that it is my responsibility to help maintain the integrity of the glove box. Print Name:_____________________________ Signature: ______________________________ Date:_____________________