Extracting iodine from tincture 20 failures in 22 attempts

[calmcatfather]

I guess today is my problem day. I have been trying to extract iodine from tincture for about 4 days. I have tried 22 times and I was only successful in 2 random attempts and I did not write down these attempts. I will write down the methods I used and the materials I used. Instead of iodine, brownish things come out in pieces. I have researched how to overcome this, I have watched videos and I am doing the same thing but I have not been successful.

- The materials I use
- %18 hydrochloric acid
- %3 hydrogen peroxide
- Sodium hydroxide
- Tincture

In some experiments, I tried adding 1gr, 2gr, 3gr NaOH to 5ml of water.

I experimented with hydrochloric acid by adding 5ml, 10ml, 15ml and sometimes 25ml.

I tried 5ml, 10ml, 30ml and 50ml with hydrogen peroxide.

I either matched the ratios I wrote here or tried adding more of one than the other. I usually strained the liquid after adding NaOH and always strained what I thought was the yellowish plastic-like povidone. I always added the hydrochloric acid slowly. and usually waited for the liquid to turn almost black. Okay, now I understand that NaOH bases the tincture. HCL neutralizes it. I still don't understand what exactly hydrogen peroxide does. It oxidizes like iron, but I couldn't figure out how. In the 2 random attempts I made, I mixed all the ingredients randomly and quickly and extracted iodine. How do I know it was iodine? After each attempt, I heated the remaining material and observed the iodine condensation. I still do not understand why brownish pieces are formed instead of iodine. Any help on this matter would be appreciated.

 

[SoldadoDeDrogas]

This is easy, I got you homie... First, let me know...

Is it iodine tincture in alcohol? %2?
Or is it povidone-iodine solution? %10?

 

[calmcatfather]

povidon-iodine solution %10

 

[SoldadoDeDrogas]

Ok. Even better. What is it a 8 or 12oz bottle? I forget.. doesn't matter anyway.
So first we will need a %25 NaOH or KOH solution in water. You'll want around 30g of NaOH to 90ml of water per bottle of I2. Add your iodine solution to a larger beaker that can hold atleast 2 or 3 times the volume.
Start slowly adding your NaOH solution to the iodine until it turns a pale yellow color. A sort of slime will develop and coagulate. You will want to filter this out of solution. Afterwards, you want to reduce your iodine/NaOH solution to about half the volume, you will need to filter out the yellow goo again. The goo is much more solid and tangible after heating. Reduce it down to about 60ml after removing all the goo.

When you have your filtered and reduced solution. Now we can get the iodine out. You will want about an equal portion of HCl acid (60ml of ~%37 HCl) to your solution. Slowly add the HCl. It will go from a clear color back to the brownish red color we started with, be careful cause it will react violently. So finally, we will need a good amount of fresh hydrogen peroxide. To your iodine/HCl solution, we want to slowly add about 4 times the volume, or about 400ml of hydrogen peroxide or until the iodine crystals start to precipitate and stop. Let it sit for a moment and stir to make sure there is no more precipitation. Decant your solution into another beaker, but make sure to use a filter to catch any iodine that may pour off. Finally you can rinse your solid iodine with some water, combine, rinse and decant/filter.

The final step if you want a very pure product, is to vaporize the iodine and get it to condense onto a cold surface and then scrape it off. You will be left with shiny crystalline iodine needles. Have you seen this technique? It is hard to explain to someone with words, but I believe nilered shows this technique in one of his videos. Basically just put the iodine in a glass and cover it and put ice on the cover, so that the vaporized iodine will condense onto the cold surface when it is heated and vaporized.

That's it, my friend. Good luck. Lemme know how it works out. o7