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Just watched a tiny pinhole leak in a cannula transfer kill an entire afternoon of work, and I need to vent before I go reset the Schlenk line.
Doing organometallic or moisture-sensitive chemistry is a completely different level of paranoia. The paper will casually say "all manipulations were carried out under an atmosphere of dry argon," but they completely skip over the two hours of flame-drying glassware, degassing solvents, and praying your septa don't degrade mid-transfer.
My personal list of inert-atmosphere misery:
Whenever I see "filtered through a medium-frit Schlenk funnel" in a paper's supporting info, I know someone spent three hours fighting a clogged frit under positive N2 pressure.
What’s the one air-sensitive maneuver or Schlenk setup that instantly makes you dread setting up a reaction?
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Regarding the last point: This is why you always have a Karl Fischer system available if you are insisting on SPS instead of properly maintained solvent stills.
Anything that is in immediate danger of exploding in contact with air, really keeps my butthole clenched
I hate any kind of air-sensitive filtration. Swivel frits are one technique I have never learned, but it's the kind of thing an expert makes look easy, that I'm sure would go south quickly in my hands.
While this isn’t air-free technique in the purest embodiment I nevertheless always get heebie jeebies when a procedure includes vacuum filtration in order to separate a solid catalyst like Raney Nickel or palladium on carbon from the extremely flammable and possibly explosive organic reaction mixture… nothing will snap a chemist out of an absentminded stupor like the sight of a shower of pyrophoric sparks threatening to repurpose their reaction mixture into a borosilicate glass fragmentation grenade & molotov cocktail combination! Be sure to never let a highly active solid catalyst run dry when performing vacuum filtration.
Organic chemist of 33 years here. I’m at the point where I just say to myself “Nope, that sounds like a lot of trouble.”
1) Having to silylate your glassware because it degrades if you don’t. 2) light sensitive and air sensitive 3) ether soxhlet (hot ether dissolves the grease on the joints)
Distilling pyrophoric metal compounds. Need such a gargantuan setup and it’s terribly sensitive.
Also, any large challenging maintenance on my glovebox gives me a scare. Don’t want to break my big expensive toys
100% cannula transfers. I did a lot of my undergrad and all of my grad work under schlenk or glovebox conditions and having a cannula clog or being worried about the tension in the needles causing trouble somewhere... Ugh