Sciencemadness Discussion Board

Mistake extracting iodine from povidone solution, what do I have.

Syn the Sizer - 18-4-2020 at 16:17

yesterday I was extracting iodine from povidone solution. I got right up to the part where it was time to filter the iodine crystals and I was too tired and went to bed, I set the solution with crystals on the bottom outside in the cold (we still have snow).

This morning I woke up and my iodine was gone. I confirmed it in solution. When I add a base it temporarily forms the characteristic red-brown of iodine in solution than a white precip, which quickly redissolves, presumably forming an iodine salt.

I tested with NaOH, NaHCO3 and cleaning ammonia, all the same results. I thought maybe it had reformed HI so I added some more 29% H2O2 and nothing.

Its a golden-yellow viscous solution and is highly acidic. I assumed the H2O2 also liberated all the chlorine too from my original solution along with the iodine so I don't believe the acidity is from HCl

Is there anyway to recover iodine or should I just bottle it up and learn from my mistake?

Edit:

The ammonia solution left a red-brown precip at the bottom of the dish but when I went to filter it the precip passed through the filter.

[Edited on 19-4-2020 by Syn the Sizer]

arkoma - 18-4-2020 at 21:33

KI from eBay much more efficient route. I have never had much luck with povidone, and it can get expensive.
*edit* link https://duckduckgo.com/?t=lm&q=i2+from+ki&atb=v1-1&a...

[Edited on 4-19-2020 by arkoma]

Syn the Sizer - 18-4-2020 at 21:50

Quote: Originally posted by arkoma  
KI from eBay much more efficient route. I have never had much luck with povidone, and it can get expensive.
*edit* link https://duckduckgo.com/?t=lm&q=i2+from+ki&atb=v1-1&a...

[Edited on 4-19-2020 by arkoma]


I do agree, this is the 2nd time I tried. The first time I didn't boil it down enough and there was still polymer left, it made a mess with the iodine when I tried to sublimate it.

This 2nd time I reduced it way down and got all the polymer out, I even has salt precipitating out. I redissolved the salt acidified and added H2O2 and there it was the iodine crystals, lazy assed me decided to go to bed and left the solution with iodine in the bottom outside in the cold until morning. Should have just filtered it, put the crude iodine in a container sealed and purified it the next day.

Now I have an acid solution and not 100% sure what it is.

I did receive 100g KI last week, the only reason I tried with povidone was I had it kicking around and thought I would give it another try.

Fery - 18-4-2020 at 23:24

Syn the Sizer - how much H2O2 did you use? Perhaps during long time your I2 was oxidized by possible excess of H2O2 into soluble HIO3.

Syn the Sizer - 19-4-2020 at 07:03

Quote: Originally posted by Fery  
Syn the Sizer - how much H2O2 did you use? Perhaps during long time your I2 was oxidized by possible excess of H2O2 into soluble HIO3.


Yes that is very possible. I was using the Nilered video as a reference. He used 500mL of 3% H2O2, I only have 29% so I used 50mL plus another about 20mL. Is it possible to recover this iodine, and if not is there something useful I can do with HIO3?

I am not to upset, sure it was a waste of povidone solution but, it was all for science and I had fun either way. As well at the very least I learnt something.

[Edited on 19-4-2020 by Syn the Sizer]

draculic acid69 - 19-4-2020 at 07:12

Is it possible it all sublimed out overnight?

Syn the Sizer - 19-4-2020 at 07:24

Quote: Originally posted by draculic acid69  
Is it possible it all sublimed out overnight?


That is actually what I originally thought, but it was under a solution and about -10C outside.

When I add a base to a test portion of the solution it starts to crash out a red-brown precip, which quickly turns white then dissolves back into solution. What I figured it was doing was reacting with the solution and forming a soluble salt. The ammonia leaves a red-brown precip behind which passes right through a coffee filter.

arkoma - 19-4-2020 at 12:46

Quote: Originally posted by Syn the Sizer  

I am not to upset, sure it was a waste of povidone solution but, it was all for science and I had fun either way. As well at the very least I learnt something.

[Edited on 19-4-2020 by Syn the Sizer]



:THUMBS UP:

Syn the Sizer - 19-4-2020 at 12:57

I was just googling HIO3. The Wikipedia page states that in a highly acid solution with an excess of Cl- HIO3 will convert into I2Cl6 which is golden yellow in solution. It will convert to I- in the presence of a reducing agent then in the presence of excess I- it will form I2.

I did a 2nd test and added way more ammonia and the solution it didn't turn red-brown like the first time, it turned deep purple almost black. I left it for a little bit and there was clearly crystal iodine in the bottom of the dish. The crappy thing is my current source of ammonia is Canadian Tire brand lemon scented cleaning ammonia.

I really believe I have I2Cl6.

Is there another reducing agent I can use or should I save the solution for some other use later?

Edit: Upon further reading I don't know if it is I2Cl6.

[Edited on 19-4-2020 by Syn the Sizer]

Syn the Sizer - 19-4-2020 at 13:01

Quote: Originally posted by arkoma  


:THUMBS UP:



Thank you, Sir.

Fery - 20-4-2020 at 01:20

Syn the Sizer - your goal is to obtain I2, isn't it? You can let react HIO3 with KI which produces I2. Do not add more KI as necessary as it would dissolve I2.

Syn the Sizer - 20-4-2020 at 07:42

Quote: Originally posted by Fery  
Syn the Sizer - your goal is to obtain I2, isn't it? You can let react HIO3 with KI which produces I2. Do not add more KI as necessary as it would dissolve I2.


Awesome, thank you very much. I just received my KI last week so I will give that a try.

Syn the Sizer - 20-4-2020 at 22:04

1 last question for this post. Is there a use for HIO3? With how easy I2 is to get should I bottle and hold onto my HIO3? I really was just doing the original extraction for fun, I don't have a use for I2 at the moment other than to have some on hand.

Syn the Sizer - 12-6-2020 at 23:58

I have decided to produce some iodate salts. I have produced a small amount of copper (II) iodate just to see the colour (very similar to copper (II) chloride. However I plan on producing 1 mole of copper (II) iodate or as much as I can to do some tests on it.