Well I am working on getting a few reagents for use in my lab and iodine was the first for me to do. I recently obtained all my equipment and am now starting on my long road.

Concerning iodine:

I did the method starting from KI and ended up with a nice mass of iodine. My question is how necessary is it to sublime the iodine or can I just store it as is after filtering it? The only thing I am planning on using it for so far is the oxidation of hydroquinone to p-benzoquinone

Thanks

~Bass

Well I dont think I will right now but I decided to put a small piece of filter paper on top of the iodine and place a little calcium chloride on top. Like a small desiccator

So in that case HI is first formed and then is oxidized back to iodine by the sulfuric acid?

Yeah, in order to form halogen acids from the halogen, you'd need hydrogen.  Or aluminum, I think that works.  2Al + 3I2 ----> 2AlI3.  AlI3 + 3H2O ----> Al(OH)3 + 3HI.  Finding a solvent that does not react with it, and is miscible with water could be hard.  Maybe just a two phase system, the HI going into the aqueous of course.  This also works for making methyl iodide if you have enough iodine laying around.

It will, but be weary, babasstone.  I have repeatedly performed oxidizing hydroquinone, without fail for many months.  All of the sudden, it will not work.  Nothing I do, makes it work.  It terminates at quinhydrone.  I immediately blamed this on my peroxide, and bought a brand new bottle of 27%.  This brand new bottle gave similar results - no crystals.  I produced some fresh iodine, and retried... Much more benzo, but still a lot of quinhydrone.  I'm starting to think I was sold bad peroxide.  The bitch is, I bought it from a pool store, and I can't go back in there saying "this isn't 27% peroxide, this is XX%" as that would bring on a whole slew of questions.  Just letting you know ahead of time, I think there might be a possibility of weird formations with wet iodine after standing for long periods of time. 

The problem with the sublimation is it seems like some of it escape out of the pouring spout in the beaker. Does a significant amount escape? I might just attempt the synth when my peroxide gets here and if nothing happens then I will sublimate and then dry it

Beeswax is always in the butter zone Douchermann.

Yeh just check out the arts and craft stores, They have large blocks of it for cheep in the candle making sections. It has the consistancy of stiff playdoh.

An easy way to get I2 from tincture or salts is to dissolve in water if not already liquid. Take about ten percent of what you have and set it aside, then acidify the rest until the PH is under 7. (I'm not aware of a reason to be conservative in this.) Then add ordinary laundry bleach a little at a time with stirring until you see crystals starting to form in the liquid. When the liquid loses most of it's color filter out the crystals and wash several times with distilled water. Wearing gloves, carefully fold the filter paper and squeeze out as much water as you can, then wrap the remaining filter paper all the way around forming a little pouch. Wrap this in several paper towels, then again with a piece of an old towel or a rag. Put it between two blocks of wood and squeeze it in a vice for about twenty minuters. If you don't have a vice just put it on the floor and stand on it. Jump up and down, side to side, and wave your arms while singing something annoying. It should be quite dry by the time you finish with the vice, or if you took the other route it should be fairly dry as long as you hit some really high notes while singing.

(Just kidding about the high notes.)

To sublime, pour it into a erlenmeyer flask. Take a test tube and wrap the top near the opening with clean rubber from an old inner tube until it fits snuggly in the flask opening, then cover the rubber with teflon tape and secure with a small piece of electrical tape. Fill the test tube with ice and insert it into the flask and apply low heat. As the ice melts in the test tube remove the water with an eye dropper and replace with more ice. You'll be able to see when all the I2 has sublimed because a clear area will form at the bottom of the flask and start creeping up the side as the heat rises. That's when you take it off trying not to shake it up, until you have it over the container you will store it in. Scrape it loose and you're done.

Vesp, I've never heard of subliming with H2SO4 but it sounds like a great idea! Normally nothing makes a bigger mess then trying to sublime wet I2. That's the best suggestion I've heard to avoid it.

HI is not so easy to make, at least not in usable concentration. There are several workable ways to do it with phosphoric acid, etc. H2SO4 will reduce it almost as fast as it's made, as will HCl.

PP