Differences

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--- glovebox [2019/06/12 10:34] – [General rules] scholma
+++ glovebox [2023/03/21 14:29] (current) – scholma
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 ======Glovebox======
+{{:glovebox.png?nolink&400|}}
 The Glovebox is located on the 7th floor of the Huygens in HL713a.\\
-The manual can be found here: {{:ilab_user_manual_final_6-7-13.pdf|}}
+The manual can be found here, it's recommended to read chapter 5: {{:ilab_user_manual_final_6-7-13.pdf|}}
-{{:glovebox.png?nolink&400|}}
 The glovebox is capable of keeping O<sub>2</sub> and H<sub>2</sub>O levels below 1ppm. O<sub>2</sub> and H<sub>2</sub>O levels can be read out on the display on the top right. The system is equipped with a large and small antechamber, a gas purification system and vacuum pump to minimize concentrations of  O<sub>2</sub> and H<sub>2</sub>O inside.
 The box is kept at a 5mbar N<sub>2</sub> over pressure to prevent leakage from the outside into the box. (If the gloves are not pointing horizontally this indicates there is no proper over pressure inside).
+The box can be operated with continuous cycling through the purifier column, for this the blower has to be on. Make sure the blower is turned off when purging.\\
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 Clean your items before bringing them in the glovebox.\\
 Discuss your experiments with other glovebox users to avoid cross contamination.\\
-Flush the antechamber 3 times when loading and unloading to prevent O<sub>2</sub> and H<sub>2</sub>O contamination and unwanted chemical release respectively.\\
+Flush the antechamber 3 times when loading and unloading to prevent O<sub>2</sub> and H<sub>2</sub>O contamination and unwanted chemical release.\\
 At all times it should be prevented that sharp objects are lying around, there's a high risk of piercing the gloves.\\
+The gloves have a maximum reach inside, do not store stuff out of reach.\\
 Clean up when done, bring in a new white solid waste trash can when full and remove old.\\
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+====Using the antechambers=====
+When possible use the small antechamber. Do not use the antechambers for storage.
+===Small antechamber===
+The antechamber can be opened from the inside or outside when it's on atmospheric pressure. The pressure can be read out on top of the antechamber.\\ Always leave the antechambers evacuated with the evacuate valve closed.\\
+Make sure antechamber is closed at the inside of the glovebox.\\
+Turn black valve to "EVACUATE" to remove unwanted chemicals from the antechamber.\\
+Turn black valve to "REFILL" antechamber will be filled with N<sub>2</sub>, fill to atm. pressure\\
+Do this at least three times to minimize contamination.\\
+Open antechamber and load, close antechamber.\\
+Evacuate, Refill, do this at least three times.\\
+Fill to atmospheric pressure, open antechamber from the inside.\\
-====Using the antechambers=====
+===Large antechamber===
+The principle for the large antechamber is the same as the small, but there is not one valve for the evac/refill but two separate valves.
+====Flushing/purging=====
+During purging the gas in the box will be replaced with the inert purge gas. Our box is connected to N<sub>2</sub>.\\
+Purging should be done when a large amount of solvents are evaporated inside or when H2O and O2 concentrations are high (>1 ppm).\\
+Always turn off the blower before starting the purge.
+Open the red valve on top of the glovebox, the system will try maintain the pressure in the box by letting in inert gas. Do this for 15min or so depending on the contamination you expect inside. Purging can also be done for hours if the contamination is large, but keep an eye on the pressure of the gas cylinder.
+====Working with thiols====
+Thiols are the sulfur analogue of alcohols, due to the sulfur thiols can have a strong odor. When taking out used glassware or bottles that have thiol contamination they should be properly cleaned. Cleaning with IPA or water is not sufficient. There is a bleach solution in the glovebox (10 parts water 1 part Glorix), bleach will break the thiol molucules.
+====Regeneration=====
+From the manual:\\
+"The purification column contains a mixture of copper-based catalyst to absorb O<sub>2</sub> and molecular sieve to absorb H2<sub>O</sub>. Over time these materials become saturated and no longer able to absorb the O<sub>2</sub> and H<sub>2</sub>O. The regeneration process allows these materials to be returned to their original state, enabling them to continue removing O<sub>2</sub> and H<sub>2</sub>O."
+  - Purge the system to less than 50 ppm of O2.
+  - Connect a cylinder of regeneration gas (forming gas) to the regen gas connection on the lower right side of the Glovebox. The regeneration gas must contain 3- to 7% hydrogen with the balance being nitrogen or argon.
+  - Ensure that the connections are tightened correctly.
+  - Open the cylinder and set the regulator to 7 psi.
+  - Turn off the blower. The column valves close automatically. There is a yellow indicator pin that protrudes from the top of the column valves. This pin recedes into the valve after it closes.
+  - Enter the Regen Control screen and press START. The regen gas begins to flow through the column and out of the regen exhaust line.
+  - Adjust the flow of the regen gas by using the flow meter on the right side of the Glovebox above the regen gas connection. Set the flow to 25-30 scfh.
+  - Press YES at the “Is Flow OK?” prompt. The regen starts.
+  - A regeneration takes 14.5 hours to complete. After the regen completes, turn ON the blower to resume normal operation.
+====Changing gas cylinder====
+Working with high pressure gas cylinders should only be done by technicians!\\
+Make sure full cylinder is ready to go.\\
+Close connected gas cylinder\\
+Open reducer\\
+Open vent valve on top of the glovebox (large red handle) to empty the gas line\\
+Check pressures on the reducer are zero\\
+Close the reducer\\
+Close vent valve\\
+Close cylinder\\
+Unmount reducer from gas cylinder\\
+Mount reducer to new gas cylinder\\
+Make sure reducer is closed\\
+Open gas cylinder with angle key\\
+Open reducer and set pressure to 5 bar\\
+Open vent valve completely to initiate automatic purge\\
+Check 0<sub>2</sub> level\\
+Done\\