Sciencemadness Discussion Board


scienteriffic - 10-12-2003 at 19:12

Hello everyone, first post here..

I have been making iodine crystals with a tincture of iodine. The method I have been using is heating the tincture and allowing the alcohol etc. to evaporate, and the iodine crystals forming on the bottom of a jar full of ice held above the heated tincture.

I was wondering how different the crystals would be if I were to use betadine/povidone-iodine. I know that the povidone was added to get rid of some of the side effects of iodine like staining, and irritation. But how different would the end result of crystals be?

Thanks in advance for the help.

DDTea - 11-12-2003 at 11:42

From evaporating the alcohol from Tincture Iodine, wouldn't that give you more Potassium Iodide than actual Iodine crystals?? A better way to get Iodine crystals would be to add a few drops of Sulfuric Acid to the tincture, then some NaOCl or KMnO4 (or whatever strong oxidizer is on hand)... Then to pour the whole thing into a large volume of water so that the Iodine crystals will precipitate.

It's the same concept as making Chlorine from HCl + NaOCl, but with Iodine instead:

KI + H+ --> HI + K+
2 HI + NaOCl --> I2 + NaCl + H2O

Not positive about the second equation, but the point is elemental Iodine will be a product of this reaction.

Omega - 11-12-2003 at 16:25

what percent sulfuric acid?

Mumbles - 11-12-2003 at 16:34

I'd say 90%+ as it will be diluted by the tinture. I wouldn't think that a lower concentration would be needed as theres no risk of over oxidation. Granted you'll probably get a little Acetaldyhyde or Acetic Acid from the Ethanol in the tinture, but you just want the I<sub>2</sub>. I suppose a smaller concentration could be used, but use a larger amount, like a mL maybe.

Potassium Iodide

Armin - 14-12-2003 at 09:44

If you had just potassium iodide and water solution would you only need to add H2SO4?

[Edited on 14-12-2003 by Armin]

unionised - 14-12-2003 at 11:25

No, you still need an oxidant.

Darkfire - 14-12-2003 at 21:02

I used h2o2 for this, at 3%, came out fine however some iodine remains in the solution.

Acid Test - 8-1-2004 at 09:59

I would think that using HCl or some other
acid would be safer than a sulfuric compound.
Especially if making drugs for recreational use.
Use acids like HCl,Nitric Acid,or
Tartaric acid/citric acid if making LSD.
It is much safer.
You can buy these at a store which sells
wine kits.Stay away from Malic Acid.It is
trouble.It is a known reactent in making
barbituric acid

Acid Test - 8-1-2004 at 10:55

I can name a few of ALex Shulgins PIKHALS and
TIKHALS that contain iodine and iodine
What are you going to do..arrest me
For isolating a new isolate from urea
and reporting it to the Sweden Pharmaceutical
industry and the Minister of Justice?

DDTea - 8-1-2004 at 11:53

I believe what he meant, Acid Test, is that talk of drugs had no relevancy here. If you have something interesting to present on the subject, we're more than happy to read it nicely compiled in the Bioactive Materials section. Here, we are simply discussing how to get Iodine from Tinctures or Povidone/Betadiene. The part of your post that most related to this subject was :

I would think that using HCl or some other
acid would be safer than a sulfuric compound.

Everything else was pointless. I don't want to develop bad feelings between the two of us. I would like to be your buddy just as much as anyone else; I'm just showing you your errors, and I hope you take it well :)

guaguanco - 8-1-2004 at 12:43

Originally posted by Acid Test
Stay away from Malic Acid.It is
trouble.It is a known reactent in making
barbituric acid

Wrong again. Esters of *malonic* acid are used to create barbiturates.

povidone is shit

navarone - 29-1-2004 at 15:28

hi guys im brand new here.
i also try to extract iodine from betadine.
i discovered that povidone is not soluble in toluene and xylene.
so i managed to separate the two.
i loaded a test tube with 10 ml of betadine,
added a few drops of water because the betadine is so dense.
i added 15 ml of toluene on the top and really gently heated it with a candle.
the temperature of the bottom of the test tube should be just enough keep ur hand on it for a few seconds.
i mean the candle has to be pretty far.
if done gently...the result is a bottom layer with a white cluody colour.
and a top layer with a clear violet colour.
none of the liquids has to boil.
now im not that good in chemestry...but whats inside the top layer.
of course i know its iodine...but which ion.
i putted the solution on a whatch glass and let it evaporate in the oven at 100 c.
the result is a brown solid from a violet solution.
so i tryed to let it evaporate at room temperature.
still brown.
i seriously need ur help guys.
how do i get pure i2 out of the toluene violet solution.
please help:(

does this work?

navarone - 30-1-2004 at 10:05

oknow managed to separete the iodine from the povidone.
but i dont know which iodine is mixed up in the toluene.
so does this work:

i? + H2O + NaOCl --> i2 + NaOCl + H2O

the result is a dense white salt that taste exactly like tablesalt.
now is that the taste of iodine crystal or i managed to deoxidise the sodium hypochlorite?
whats in the crystals?

Geomancer - 30-1-2004 at 16:09

That wouldn't be I<sub>2</sub> then. I've just resublimed a small amount of iodine frome tincture (unfortunately, the crystals are somewhat damp). At room temperature, the element forms dark purple (almost blackish) crystals with a distinct metallic luster. The material emits purple vapors that are distinctly visible in the bottle you store it in. Altogether a visually pleasing element. The odor is also somewhat distinctive, similar to chlorine (you feel as much as smell it) but with a pronounced earthy component.
Wear gloves when handling.
Heating at 100C would have evaporated any free iodine you had. Rhodium has a page on isolating from povidone; I'm not sure if it's trustworthy. Hypochlorite is not the best oxidant to use, since it is basic and some of your product will be tied up in hypoiodide. Better to add some acid and oxidize with chlorine (don't overdo it or you'll get an interhalogen). Better still is to use H<sub>2</sub>O<sub>2</sub>.

chemoleo - 30-1-2004 at 19:23

Actually, iodine makes very very nice crystals. A few weeks ago I presented a metallic looking crystal to my boss, claiming it was the crystal of my protein (as mentioned before I am working on protein structures right now) - he was really impressed at first but realised right away that this was a joke - of course protein crystals look very different to iodine crystals.
Anyway, I kept those iodine crystals (about 15 mm long) outside, and after one day the crystal had shrunk from a metallic defined 'colour' to a dull piece of junk (which didnt resemble a crystal at all)- so be warned, it really sublimates.
Nonetheless, if you ever get hold of solid elemental iodine - keep it in a lidded flask. Heat it up a little (like putting it on top of a radiator) , and wait for a bit. YOu will find beautiful crystals of iodine. It is very impressive.
Just that fact alone should give you an incentive for making elemental iodine!

navarone - 31-1-2004 at 01:56

so whats in the toluene is i2 right.
so ur telling me to put a few drops of h2o2 and leave it to evaporate and ill get i2 crystals?
hmmm... ill try.
what is brown iodine?
is it i2 or another ion?

so since now i did.

loaded them test tube with tincture water and toluene.

heated it until the lower layer becomes cloudy white.

separate the 2 layers.
let the toluene with violet color evaporate

and the result is a brown crystal.

would h202 make the difference?

do ihave to make it evaporate under heat or in the freezer?

will distillation work?

navarones ghost - 12-2-2004 at 16:52

hello everybody.

aight...iodine sublimises very easely even at room temperature.

if it does so even when solved in liquids...
distilling would do the trick.

once i boiled the betadine mixed with the equal amount of water and the mixture turned almost white.

so i guess the iodine just flew away.
if it did....distilling would work.

the problem is....will the i2 turn into i- or i3- when distilling?
please let me know aight?

(to those who respect me)