Ammonium Tri Iodide

[DandyGurl]

Ok I am trying to make some from house hold ammonia, and 2% tincture of iodine. I put it on a coffee filter, and can get it to turn black, but it seems the amonia, evapoates and the crystal break down as a purple hue forms around the edge of the filter. Or where can I get iodine Crystals...

[budullewraagh]

i take it you mean nitrogen triiodide. you cant do it with tincture. acidify the tincture with sulfuric acid, then add a strong oxidizer (try some conc hydrogen peroxide) and recover the iodine crystals.

 

iodine crystals are really expensive so just try obtaining them with the tincture.

 

as a side note, do not make any more than 2mL of this at a time, lest you die. nitrogen trihalides are incredibly unstable and are usually detonated by a slight air movement.

[DandyGurl]

i take it you mean nitrogen triiodide. you cant do it with tincture. acidify the tincture with sulfuric acid' date=' then add a strong oxidizer (try some conc hydrogen peroxide) and recover the iodine crystals.

 

iodine crystals are really expensive so just try obtaining them with the tincture.

 

as a side note, do not make any more than 2mL of this at a time, lest you die. nitrogen trihalides are incredibly unstable and are usually detonated by a slight air movement.[/quote']

Thanks for the help I made some before with crystals, we had three piles with in a sq foot. We threw a pea sized paper at one pile and they all went off!!!! Neat stuff...

[DandyGurl]

i take it you mean nitrogen triiodide. you cant do it with tincture. acidify the tincture with sulfuric acid' date=' then add a strong oxidizer (try some conc hydrogen peroxide) and recover the iodine crystals.

 

iodine crystals are really expensive so just try obtaining them with the tincture.

 

as a side note, do not make any more than 2mL of this at a time, lest you die. nitrogen trihalides are incredibly unstable and are usually detonated by a slight air movement.[/quote']

Where can I get concentrated H2O2? The stuff at the store is like two percent. What molar H2SO4 should I use? Do I evaporate the solution to yeild Iodine crystals? Or do I mix all with amonia, and let dry?

[budullewraagh]

for your peroxide, look online, or better yet, go get 3% at a pharmacy and fractionally freeze it. your peroxide should freeze at -11 celsius, while your water will freeze at 0. use 20-40% sulfuric. dont even try to evaporate the solution, as you will die. you will have to be careful with the molarity and volume of your sulfuric and peroxide. if you aren't careful, you will get peroxymonosulfuric acid, which is not to be messed around with because it detonates easily and will rip through your flesh with haste (hence its nickname pirahna bath). do not add your ammonia until after you recover your crystals. to recover your crystals use a solvent. be careful, as isopropanone will yield AP, which is also very unstable. also, be careful when working with carbon chlorides, as you just may end up with phosgene or a similar compound. also, alkanes are no good, as they will explode.

[DandyGurl]

for your peroxide, look online, or better yet, go get 3% at a pharmacy and fractionally freeze it. your peroxide should freeze at -11 celsius, while your water will freeze at 0. use 20-40% sulfuric. dont even try to evaporate the solution, as you will die. you will have to be careful with the molarity and volume of your sulfuric and peroxide. if you aren't careful, you will get peroxymonosulfuric acid, which is not to be messed around with because it detonates easily and will rip through your flesh with haste (hence its nickname pirahna bath). do not add your ammonia until after you recover your crystals. to recover your crystals use a solvent. be careful, as isopropanone will yield AP, which is also very unstable. also, be careful when working with carbon chlorides, as you just may end up with phosgene or a similar compound. also, alkanes are no good, as they will explode.

Ok now I'm starting to understand...

Bare with me her im just a stupid girl with a few years of chem....

Whats the formula for peroxymonosulfuric acid? H2SO2 ? Dont have my periodic table handy...

 

1. freeze the water out of my H2O2

2. Mix H2SO4 and H2O2 ( what molar H2SO4?) and in what ratio? Should I add my tincture to it at the same time? Will the crystals be able to be filtered out?

[DandyGurl]

AP= ammonium percholrate?

[budullewraagh]

Whats the formula for peroxymonosulfuric acid? H2SO2 ? Dont have my periodic table handy...

haha, no, it's [math]H_2SO_5[/math]

 O

 ||

H-O-S-O-O-H

 ||

 O

 

2. Mix H2SO4 and H2O2 ( what molar H2SO4?) and in what ratio? Should I add my tincture to it at the same time? Will the crystals be able to be filtered out?

add the sulfuric (20-40%) to the tincture, allow it to diffuse for a moment, then add the peroxide. crystals will appear. remove the crystals using a solvent.

 

AP= ammonium percholrate?

haha, no; it's acetone peroxide, which is infinitely worse

[DandyGurl]

haha' date=' no, it's [math']H_2SO_5[/math]

 O

 ||

H-O-S-O-O-H

 ||

 O

 

 

add the sulfuric (20-40%) to the tincture, allow it to diffuse for a moment, then add the peroxide. crystals will appear. remove the crystals using a solvent.

 

 

haha, no; it's acetone peroxide, which is infinitely worse

 

What solvent do you recomend? somthing nonpolar?

[budullewraagh]

oh certainly something nonpolar. just be careful, as you really dont want to make organic peroxides. i bet glycerol would work well

[jdurg]

It might be easier to just heat the tincture up and collect any iodine vapor on a glass plate with ice on it. This will give you pure, very fine, iodine crystals from the vapor. If you want to get the iodide ions to convert into iodine, you could just generate some chlorine gas and bubble that through the iodide solution, and then collect the iodine by heating the solution and collecting the crystals on an ice-cooled plate.

[budullewraagh]

im sure she wants to oxidize the iodide; your yield (almost) doubles. with regard to the chlorine method, that's a good idea, although you may have a problem, as if you lack sufficient tubing, you will end up with a great deal of chlorine not oxidizing your iodide and you will need a few moles of it to work. if you have tubing that works, however, you're set. also, you may want to heat your reaction vessel if you do this

[DandyGurl]

What about pure tolulene as a solvent?

[budullewraagh]

i suppose it would work...altho it would be a bloody poor waste of toluene. where do you get toluene???

[Gilded]

"where do you get toluene???"

 

I thought you can get toluene from just about any of those bigger paint stores? Or is that some sort of mix instead of pure toluene?

[budullewraagh]

i hate where i live. we can't get anything here. at all. the only form of oxidized chlorine we can get is Na/Ca hypochlorite. no chlorates/perchlorates (except that incredibly small amount in caps/match heads). no nitrates, save like 3% mixed with a bunch of other trash. no sulfuric except in car batteries. almost no hydrochloric even. no organic precursors. bah i hate it.

[premjan]

paint stores might sell turpentine. toluene?

[r1dermon]

when extracting the H2O2 via the freezing method, i suggest a sponge. it gets to be a slushy mix. the H2O2 doesnt really fully extract, its just mixed in with a bunch of ice crystals. just squeeze a sponge and press in hard into the mixture and then let it soak up the H2O2. worked well for me. wear gloves;)

[Gilded]

"i hate where i live."

 

Yet you live in US, the homeland of United Nuclear and other fun... stuff. >:/

[budullewraagh]

i will say that i enjoy my unitednuclear stuff. not particularly cheap tho.

 

actually, i have a great way to fix that; i found a bunch of people that are giving away grants. apparently i should be able to get $5k if i try hard at all :):)

[boris_73]

also in america the prices are very cheap compared to england, saying that thats not hard to beat

 

Edit: also i would just like to say there was a whole post on how to extract iodine crystals from seaweed, that might be a better method

 

Edit2: heres the link for it http://www.scienceforums.net/forums/showthread.php?t=6462

[DandyGurl]

i suppose it would work...altho it would be a bloody poor waste of toluene. where do you get toluene???

Sherman Williams. 12 bucks a gal. Pure too. I add it to my gas tank to make 114 oct race gas...

[DandyGurl]

also in america the prices are very cheap compared to england' date=' saying that thats not hard to beat

 

Edit: also i would just like to say there was a whole post on how to extract iodine crystals from seaweed, that might be a better method

 

Edit2: heres the link for it http://www.scienceforums.net/forums/showthread.php?t=6462[/quote']

Go mucking through the mud, or go to the drug store to buy tincture, Hmmmmmmm....

[Gilded]

"Go mucking through the mud, or go to the drug store to buy tincture"

 

Judging by looking at your house and car, you seem to certainly be one of those people who have the money to buy all the tincture in the world instead of running around at the beach chasing seaweed.

[boris_73]

LOL im not one for mucking through the mud either, and besides i live in Manchester quite far away from any beach or such so i would just buy my seaweed from a shop, in fact i just buy pure iodine crystals from chemical suppliers to save all the bother but making them can be quite fun