Finally, I hope. found a host for my iodine monochloride video that didn't want verification by phone number (sorry, not getting anything that can identify me
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IClfinal.mp4 its a download rather than a direct link, about 86 total)
This installs a toolbar, just delete it after asap, was the only place that didn't ask for ID of some sort.
Just thought I'd warn you. File is .MP4, has had the metadata removed, so windows media player won't play it. VLC media player is free and it doesn't have any issues.
Notes-If following my synthesis, do not retain the no-hole stopper whilst passing Cl2 or other gases through the drying agent/iodine, otherwise pressure WILL build up and force a joint apart, whichever is weakest, resulting in the venting of Cl2 through the system to the atmosphere. This was placed in there to avoid anything volatile evaporating, such as the iodine, and escaping. It seems however, save to SLOWLY pass Cl2 through the system even so, given it reacts with the iodine to form a liquid, or in the case of excess Cl2, either through I2 or ICl, to form the trichloride, ICl3. This can be done by adding HCl and hypochlorite via large syringe, such as a 60ml oral/enteral medical feeding syringe without a needle attached to a short length of rubber hose, using a distillation adapter to connect the Cl2 generator to the liebig condenser, and a short length of rubber hose, serving to mate the syringe (clamped whilst attaching the syringe and during its removal to refill), during the synthesis itself however, a stopper with one hole and a long piece of glass tubing, attached first to a suckback trap (I superglued a one-way valve and seal to a medicine bottle cap, just to prevent water suckback into the iodine monochloride accumulating in the receiver, this would be disastrous, certainly damned unpleasant, since it would hydrolyze the product back to iodine and chlorine gas, and a little would produce a lot of toxic gas.)
A respirator with a cartridge suited to acid gases and halogens is REQUIRED, ICl is highly toxic, more so than chlorine gas.
Use teflon and if grease is to be used, use a perfluorocarbon grease, since ICl is a STRONG oxidizer and will reduce the likes of dow-corning high-vacuum grease, or petroleum jelly to the consistency of set cement, so wrap stoppers in heavy layers of teflon tape and perfluorocarbon grease both under and over them, likewise any glass to glass joints need such treatment because should you try and unstick a jammed stopper and get this stuff on you, I shudder to even contemplate what it would do to flesh. Don't use metal vessels to transfer or store it, it will eat through them. It does not attack glass, but DOES attack plsatics, viciously so, also the vapor can slowly permeate through plastics. Outlet gases and vapors should be led through a suckback trap, and then into a solution of saturated sodium, potassium carbonate etc. AFAIK it decomposes in carbonate, although not bicarbonate, to iodates) hydrolytic decomposition is violent and rapid. i've only added drops at a time to water to test how quick this occurs and it is instantaneous, a little puff of green Cl2 gas given off and iodine sinking to the bottom of the water. A large quantity of this compound would, most certainly, result in a correspondingly large release of chlorine gas, and quickly. Not desirable, not pleasant, not safe.
Needless to say, you don't want this happening in your lungs or eyes, WEAR A FUCKING MASK AND FACE SHIELD, with goggles underneath the shield, and long, elbow-length gloves. ICl is HIGHLY TOXIC and can also be ABSORBED THROUGH THE SKIN, affecting the kidneys as well as the lungs. No, it wouldn't make a good kitchen spice
I can't stress enough-FACE SHIELD covering FULL FACE, the more the merrier. You wouldn't get chance to react it this got in your eyes, chances are instant blindness would be the result. Not to mention it would hurt like fuck. Oh, and turn to acid while it broke down in the tear fluid. On skin, SEVERE burns, near instantly. Chances are they would be deep burns, up to third degree. Easy synthesis, lots of safety precautions needed and great care taken with the procedure.
Some notes as to the video-second little part of the sections spliced together got repeated, ignore that, video looks good.
I said during one early part that the medical air pump was being used to drive the Cl2, this was a momentary lapse of narration, its argon from a tank being used for this, the medical air pump is in fact plugged into the liebig condenser with the drying agent (closest to the right-hand flask) to pre-cool the Cl2 gas before it enters the water-cooled condenser packed with I2)
The beginning of the rxn can be seen when the orange color forms, this is where the chlorine first meets the iodine, and a little iodine TRIchloride forms (a reversible rxn) the monochloride is a dark, bromine-like liquid of low melting point (two melting points actually depending on whether its alpha- or beta-ICl formed, the alpha crystal form gives long needle-like crystals when solidified, the beta form gives rhombohedral plates). Oddly, it can supercool from the looks of it, remaining liquid even when immersed in cooling baths of things like ice-ethylene glycol or diethylene glycol, acetone and methylated spirits with a little water and salting the ice, this gives a sub-zero temperature, yet nevertheless, I have personally seen ICl remain liquid despite this, and despite it being colder than its melting point.
To contain ICl, keep it out of light for prolonged periods, brief exposure such as to open a bottle and use some of the reagent is alright, its air-sensitive and moisture sensitive (atmospheric water content included), preferably backfill the bottle containing the ICl with argon or nitrogen for storage, wrap the screw-thread of the bottle with teflon tape, and use a bottle with a teflon cap and a resistant seal. In such a bottle, the ICl I made, I still have, in good condition without any noticeable hydrolysis.
ICl3 on the other hand, should be stored under an atmosphere of dry chlorine gas, for it is, I believe, unstable under an air atmosphere and I am not entirely sure about under inert gas. Excess chlorine should be used as the atmosphere of the bottle in order to prevent decomposition. Not done anything myself with ICl3 yet. DO NOT let it contact METAL POWDERS, risk of spontaneous ignition, and certainly one small flame and it'll burn instantly and intensely) bulk metals, E.g iron bar, etc. etc. would just corrode rather than burst into flames. Phosphorus (red) is hypergolic with ICl, the very moment the two contact, such as one drop falling on red phosphorus powder, the RP instantly ignites. Haven't tried it on white phosphorus but its even more reactive than the red allotrope, the reason I haven't, is that whilst I have most of whats left of 2kg red phosphorus on my lab reagent stockroom, I have only a small sample of white phosphorus, and I don't intend on just burning it for no gain. There isn't the slightest doubt that it would burst into flames, since ICl is a strong oxidizer.
Oh and don't use plastic keck clips, because even heavily wrapped in teflon tape, and greased to fuck, then wrapped again, they without exception, disintegrate just from the traces of ICl that manage to make it out of the glass fittings. This happens quickly indeed, You'd be lucky to have one last a full hour before disintegrating or cracking straight through, and whilst I've not tried it, the only solvents I'd trust, are highly inert ones, such as fluorocarbons, dichloromethane, carbon tetrachloride, or possibly chloroform. ICl eats things. even the lawn around the table the apparatus is set up on is now bleached pale yellowish white (over time). Likewise don't do this in the rain, you really do not want ICl or ICl3 getting in contact with water.
And where my voice changes, those are just momets when I need to wear a gas mask,
If intending to produce solely ICl rather than ICl3, there is a little trick, that being to use excess I2 in the iodine column, and any ICl3 (yellow-orangey solid) formed can be left overnight, the excess Cl2 or/and ICl3 reacts with the excess iodine to reform ICl after leaving the setup overnight. Iodine isn't too cheap, especially due to the high atomic weight of iodine, so the less wasted the better, Those streaks of ICl3 in the I2 column reverted on standing overnight to give ICl once again)
In bright weather, cover the receiver pluss the I2 column with tin foil just to keep out the light and enhance stability of the monochloride.
It adds to alkenes (olefins, carbon-carbon compounds containing a C=C double bond) like for example, bromine does, forming in this case not a mono or dibromide, but a mixed iodobromide where one of the halogen atoms adds to one end of the double bond, and one to the other, this inclides substitution on a cycloalkene ring. Alexander 'sasha' Shulgin, rest his great soul, also used I found out later after making the reagent, iodine monochloride as the iodinating agent in his sytheses of DOI and 2C-I (2,5-dimethoxy-4-iodoamphetamine and 2,5-dimethoxy-4-iodophenethylamine) respectively. ICl was used .
So, enjoy, folks.
