SellaTheChemist
Saturday. My glove box remains dead after a mysterious cockup while I was on holiday that caused one glove to be torn and the catalyst to sinter into multicoloured lumps. It doesn't get much worse than that!
But after several abortive attempts to fix things, I woke up at 02;30 in a cold sweat about it. And then a possible solution dawned. So, back to the lab to try it out.
That glovebox has run for 30 years on the same catalyst. I'd hate to lose it. #chemistry #InInsomniaConsilio
botvolution
@sellathechemist I need to know more about very sensitive organometallic compounds used as indicators
SellaTheChemist
I return to my #glovebox to discover that the catalyst heated but the gas did not flow through at all - the flow rate seemed correctly set at the start. Does this mean that there's a deeper problem still lurking?
A whole day wasted. I'll have to try again tomorrow. Fingers crossed.
SellaTheChemist
#GloveBox Saga. So the regeneration cycle is on for the catalyst on my #glovebox. Because I'm out of town I've got a couple of students primed to take photographs of solenoid valves to see whether the lights go on in the right order and whether when VRE opens the gas actually flow. If the light is on but gas doesn't flow then it's back to ordering another replacement part. How many weeks might that take? #sigh #chemistry #academiclife
SellaTheChemist
And so my glove is is undead!! Atmosphere well below 5 ppm of oxygen. Now the cleanup begins.
The spots are a very sensitive organometallic compound used as an indicator. Green is good. Orange is baaaaaad. #chemistry #academiclife
SellaTheChemist
After multiple vicissitudes the correct replacement circuit breaker for my #glovebox has finally arrived. When it was installed, the blower that runs the recirculation in my glove box came back to life. 🍾🍾🍾 So now I need to purge the box with a cylinder of nitrogen and regenerate the catalyst which I have completely replaced. It's been a 2 ½ month emotional roller coaster. Fingers crossed we'll have the atmosphere down around 5 ppm O2 before the end of the week. #chemistry #academiclife
SellaTheChemist
#Glovebox purged with 100 bar (7 m3 of nitrogen). Now the catalyst is heating up waiting for its nitrogen/hydrogen feed to reduce it down and activate it. We might have a working box by morning.
And then the shite jihad will begin. Time to clear out a lot of ancient samples and abandoned schlenks. There's a fair bit of rather manky white phosphorus and alkali metal in there so there may be some fun to be had… #chemistry #academiclife
SellaTheChemist
@botvolution It's a reduced titanocene. You mix two spatula tips of red titanocene dichloride with one spatula tip of zinc in dry toluene under nitrogen. You then stir it for a day or so and the solution gradually goes green as the zinc dissolves, throwing its two electrons at two titaniums. The result is a beautiful deep green trimetallic complex that is very sensitive indeed. You put a spot down and wait for the solvent to evaporate. If it stays green you're set! If it discolours… #sigh
botvolution
@sellathechemist
After a bit of goo-gerling I think this is for detecting O2 ?
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