Found that a stuck 3-neck flask connected to a still head was freeable at the point the still heads female joint was plugged into a pair of condensers, heavily wrapped in teflon tape to prevent attack by what was in the flask.
Managed to get the two apart, so quickly put them back together, gently (the contents, a fair quantity of iodine monochloride, around 40g are sensitive to air, and react with water, potentially violently, ICL gives off some extremely noxious fumes, that are highly corrosive to many organic materials, including many plastics. It is a solid at low temperatures, but at room temperature a quite volatile, reddish-brown liquid with a generically halogen-ish odor, but despite the fairly moderate freezing point seems to be able to supercool without freezing even after a month in the fridge)
Which is where I keep mine, in the fridge (not the one for food, the chemical fridge dedicated to the storage of volatiles, nasty things, and volatile nasty things (like iodine monochloride), in a chemically resistant bottle, the cap made of some very resistant plastic, teflon or some other fluoropolymer I guess. Filth left them behind after a raid based on a bogus warrant. Ostensibly to 'take samples' which they basically just opened and exposed stuff to air that shouldn't be, put a few ml of this that and the other in these bottles, left the bottles on the bench, arrested me on a trumped up excuse which never came to jack shit due to complete lack of evidence, due to the fact that I had nothing to do with what I was falsely accused of whatsoever, and fucked off.
Presumably they need to have such containers for raiding terrorist cells and the like that could potentially hold really, really nasty shit, or anything from coca cola to VX nerve agent, so I store my ICl in one of those bottles, I've got several of them, reserved for storage of the most aggressive, toxic, hazardous etc. chemicals in my repertoire of reagents, added a good thick layer of teflon tape tightly wrapped round the screw threads of one of those bottles and keep it in my chemical fridge, well marked with the appropriate warnings lest some moron ever think about opening it inside (I got a single whiff of ICl once (well mostly, some iodine trichloride was present but its a solid and much less volatile, along probably with some chlorine gas mixed in during the reaction to make the ICl and possibly a little iodine vapor from ICl or ICl3 vapor in the air hydrolyzing to the elements, got bitten by it due to a gas mask failure, quickly repaired it but in escaping the area to do so got a breath of the ICl and it left me needing an inhaler for the next 2-3 days. So what is probably around 2 ounces give or take a gram or two would definitely NOT be something I'd want some cretinous copper etc. fucking with and letting loose in the house. So, its labelled with a big skull-and-crossbones on the cap and on the label, that it releases highly toxic fumes in air and reacts dangerously with water.)
So far though so good, its behaved itself, kept as it has been, kept cold, in its resistant bottle, purged with argon. But on opening that flask up, to my delight, ran off to get my blast shield over my face, safety gear on, gloves etc., took the plunger out of a big (250ml I think) glass syringe, removed the needle so it wouldn't either A-be melted/burnt through or B-degrade and contaminate the iodine monochloride with residues of the metal from the needle or its plastic attachment. (its not for giving injections, rather its all made out of glass, with no rubber or plastic parts so as to be ideal for transfer of extremely corrosive compounds, and doling out measured quantities of such things, as well as solvents that attack plastic/rubber)
Stuck the end of the big syringe (the barrel is nearly 3 inch wide) into the narrow bottle neck and quickly inverted the whole thing, on its side, angled so the remaining ICl would come flowing out of the distillation adapter, since I've not yet freed the stoppers. Realized there is quite a lot more iodine remaining in one of the two condensers connected to the chlorine generator, so will teflon- tape the the adapter up, make sure there is no grease on the joints (usually grease is a good idea for ground glass joints. Not with iodine monochloride. It'll turn most greases into something resembling cement, and most plastics exposed to even dilute ICl vapor disintegrate in no time-I used, or tried to use, the first crack at making it, plastic keck clips to secure the glassware. I don't have many plastic keck clips at all now. Only ones I have are the ones that never went anywhere near the ICl synthesis, the rest crumbled into little pieces or turned to dust, or else split right through)
On weighing it though, the ICl I collected today from the freed flask, I found I had at least doubled my yield, just from adding the remaining ICl in my flask. And all I need do is re-start the chlorine gas generator, after packing the drying tube section with fresh anhydrous calcium chloride and run chlorine gas over the remaining iodine in there and convert it to ICl, wouldn't surprise me if there is enough in there to triple or quadruple my yield at least
