Finally! Povidone iodine extraction (this one works way better than Rhodiums extraction method)

OK guys.
Im happy you accepted to give me another chance and i just wanted to say thanks first.
Well...to thank you guys back i want to share what i learned in my period of absence from this forum.
Something that has been complicating chemists and meth makers life, is the damn extraction of iodine from the most available source. povidone iodine.
The problem is that povidone traps iodine really strongly by a charge bonding.
povidone was designed to trap the iodine and not let it sublimate at room temperature so that people who would like forget to close the lid of the container wouldnt find the solution totally iodine free after a few minutes. Another use of povidone is to increase the solubility of iodine.
As we all know iodine is not that soluble in water but if you notes, in tinctures like betadine there is 10mg of i2 per ml.
Now how is that possible?
sice povidone is very soluble in water, the iodine attracted by it will also dissolve like sugar. So the tincture doesnt need alcohol to dissolve the iodine...it can be dissolved in common water.
now heres a pic. of the povidone iodine molecule:




So here u can see that iodine is not bonded to the povidone but its just held by some kind of charge.
Heat is the solution to free the i2 from the evil povidone.
now i know you are gonna say that there is already a method of povidone iodine extraction on Rhodium.ws.
I read it......and all i can say is that it sucks.
It sais:

1) boil your liquid to absolute dryness
2) put the dry povidone i2 in an erlenmeyer and set up a coldfinger apparatus
3)add heat and the iodine will sublimize from the povidone.

WRONG! WRONG! WRONG!

Ive been studying this extraction for pretty long so i will highlight the errors:

By boiling the tincture you will just let about 40% of the iodine to sublimize away and spread into your house.

The iodine that will sublimize from the dry liquid will be just something like 20%.

Trust me,i tried this method many times.

The sublimation tecnique is right but its not done in the right way.
So after lots of practice...i finally solved the maxi problem.
The equipment ur gonna need is:

1)liebig condenser
2)quickfit erlenmeyer(a big one)
3)hot plate or heat source

In the method that i will describe sonn there will be no need to dry the tincture.
ok heres an image of the setup:




The secret is H20 and a thin layer

the water will help iodine escaping from the povidone since iodine gets trapped immediately when it touches the povidone.
the water will keep a certain distance between the povidone molecules.
the thin layer also helps the sublimation.
I tried this experiment before with the erlemeyer half full and it didnt work that well.

I suggest to put more water than tincure for a better sublimation. But the thin layer must not exeed 1cm.

it is reccomended a big erlenmeyer to extract more tincure at the time.
I first started with a 100ml erlenmeyer and i had to extract 30mg at the time since the diameter of the erlenmeyer was so small.

Once the setup is complete just turn the heat to 300-400c' and u will start to see the iodine sublimating.
After one minute you will see a really pretty purple cloud inside the erlenmeyer and some cristals growing inside the liebig condenser.
Alot of water will come trough but it will condnse and drip back to the container.
boil the mixture until you cant see any purple gas anymore.
For a final check, see the color of your mixture.
Dont look it from the top but from the side.
he mixture should be pale pale yellow.
What does that mean my friend?
finally the iodine said goodbye to the povidone.


When all the iodine has sublimated, turn off the heating pad and trow away the povidone H20 mixture.(watch out! the erlenmeyer is gonna be hot!)

Dont u even dare putting some more tincture inside the mixture since the povidone concentration will be soo strong and the iodine will never sublimate away.

Pour the mixture off, clean the erlenmeyer and get ready for the next extraction.
You will be able to extract like a little at the time depends on the diameter of the erlenmeyer. bigger is the diameter, more tinc u can add to that 1cm layer.

After a few extractions, ur condenser will be "full" of iodine crystals sublimated on inside walls.

Now all you gotta do is to take it out, and thats a bit tricky but u can build a "pusher".

What i did worked well. You gotta need:

1)a testube cork(rubber)
2) a thin stick longer than the condenser

Calculate the diameter of the iniside walls of the condenser and cut a piece of the testube cork with a diameter slightly bigger than the walls.
Then spike the rubber piece to the long stick.

Thats gonna be perfect to push out the iodine.

Now u understand why a liebig and not an ahlin condenser must be used.
Its a bit tricky pushing the crystals out from an ahlin condenser.

A few more precautions for the pushing out of the iodine.
Put ur condenser upsidedown with a watch glass on the bottom.
push the iodine from the top and slowly since it will pop away easely and not flow down like cream.

Well...shit! this extraction method kiks ass.
From a 1 liter tincture with 10mg i2 for ml...i extracted a bit more than 9 grams.
Thats more than 90% of the total iodine inside the tincture. And then a povidone tincture bottle doesnt cost that much either.

Now i know that a cold finget could be used instead....but the problems are:

The coldfinger will cool down the erlenmeyer and make the iodine sublimize inside the walls of the erlenmeyer.
The coldfinger will be too close to the boiling liquid and there might be a fuck up!

Well finally! the problem is solved!
after many readings of hard work with failed extraction...the method was pretty easy at the end.

I hope this method will be useful to you guys. i cant wait to give this method to The-Hive. Im sure much more people will be happier there than here..lol!

peace

from >>-Navarone->

-The End-

[Edited on 18-4-2004 by _navarone_]

Amazing method!!Well, i can try this soon enough..

Dunno!

I dont know.

Where i live, betadine is the only iodine tinc available.

i dont think povidone is that difficult to make in labs.

The advantage of povi I2 is that it can be dissolved in high concentration inside water.

Have u notesed that the liquid is black.
Povidone is a white crystal so the black is the iodine and to make the water that dark it need a lot of iodine.
10mg for ml

Ki and I2 tinctures are dissolved in alcohol.
and i dont think KI is that soluble in alcohol.
Povidone iodine industries dont have to use alcohol for the tincture so that makes the tincture cheaper i think.

oh...wait a second ill go and check.
......

Hmmm i went on an italian Drugstore website:

http://www.farmaplanet.it/farmacoviewadv.asp?Nome=&Minsa...

Well.....even if nobody(or maybe someone) hee speaks italian,u can see
that a 100ml solution of alcohol with I2(iodio) and KI (ioduo di potassio) costs
5.89 euros.

A 125 ml solution of betadine costs
7.90 euros.

Im sure betadine has more iodine than the other alcohol solutions.

Betadine has a 10% of iodine in itself.
The other alcohol solutions ive read about have from 2% to 7%.
So yeah...in proportions of iodine, povidone iodine solutions are cheaper.
And i think the extraction of iodine from povidone is easier then converting KI to I2 and then sublimize it.

I wanna make a correction to the extraction post i just writed down.

The percentage of water should be higher(70%) for an easier extraction.
But remember..the layer must not be higher than 1cm or the iodine will encounter povidone molecules more frequently during its sublimation.

I just got a 4 liter quickfit erlenmeyer and its sufficent to extract 1g at the time

The duration of each extraction is 15minutes.
So i guess is totally worth it.

[Edited on 18-4-2004 by _navarone_]

You think so...

Costs

I was excited to see that someone put some thought into a feasible extraction method, however if according to your yeilds from starting weights. We would be talking over a hundred dollars just to get close to an oz? Is that right?
Apologize ahead of time if I computed your weights incorrectly but in Vegas 8oz of Povi is running almost $13 for 8 oz to get a litter a min of 3bttls for 9grms. So again times say 3? Is that correct?

Pardon my rant but this will be the first and only time that I do this since this is not the forum to do it. But Eph will never become illegal since there is to much money to be made by pharmeceutical companies. And I totally understand the hatred that is shown by legitimate chemists at the tweekers who put this current situation into motion. However I think what the biggest problem is... you have a government who's main concern was to hurt its own people by locking them up for long periods of time and not being concerned with the huge mexican trade that took its place. Where they are producing far larger numbers than any american cook even dreamed of. Yet all they face is possible deportation only to return in a week. The feds are famous for misinformation and promoting fear. They did not affect the fact that meth is still the #1 drug within the US but changed the means of its accesibility. Taking money out of the american cycle and laying it down outside of our borders. Now that is intelligence. It reminds me of the commericals that ran a few years ago about how puchasing this illegal drug from american cooks was funding terrorist yet the only person I knew that was being funded was 7-11's,home depots, and wal-marts . But can you say that know when most of this money is being diverted to a country which is so based in poverty that it doesnt care who it goes to bed with. I myself am amazed by science, I will never be as smart as some of your contributors that I can admit. But with this intellegence I see sometimes lacking of common sense. I mean that with no offense. I can never justify the actions of many of these people. But isnt the point of science- the desire to understand things, carrying it out through experimentation, and the such. This does happen in many ways legal or otherwise. Its always easier to say that what you do is perfectly ok its the other people that have the sickness. But I think thats just a little bit too judgemental.
Again sorry to be wasting your time, but I just had to get that off my chest being that at one time or another I have been on both sides of this fence.

Sorry to be a killjoy, but in terms of economic feasibility, I'd have to suggest (if KI is not an option and it ain't anymore, least hereabouts), then it might be worthwhile purchasing Kelp - you can buy it by the metric ton, it is not regulated, is available at mild markups from hippy stores and contains appreciable quantities of iodine.

Insofar as separating PVP & I2, I'd pretty much have to suggest that you read up on what happens to PVP when it's solution is mixed with phosphate salts (ie. it salts out pretty rapidly according to the lit) - which might be of some use - given that it would make the isolation & drying of the PVP-I2 rather simple. Once you have the problem nice and dry, it might be worthwhile looking into what organic solvents I2 is soluble in and which ones PVP ain't (and vice versa). Soon as you find one that one is freely soluble in and the other ain't, I suggest you race back here and tell us about it, I'd suggest maybe pentane/hexane/etc.

The lit also says that PVP is liable to cross-link when exposed to protic acids, which renders it insoluble in water. If you oxidise I2 to iodate it will go yellow, addition of aluminium (like a suitable, ACS reagent grade, pull-tab off a drink can) will see the iodine given off as a gas, ready to condense on any suitable surface, like your eyes, skin, roof, or perhaps even a coldfinger. Or so I was once told by someone I met long ago (they found out by overoxidising KI with OCl till it went sulfur-yellow).

Iodine from providone-iodine?

oh sh*t

Quote: Originally posted by len1

Unfortunately KI is not an option here, as its in the same class as I2. If the US restricts I2, KI must surely follow - those who can use I2 for illegal purposes, should have no problems with the high school oxidation of I-. Unfortunately the restriction on I in any form is just about the only effective 'precursor control' theyve come up with because theres no high concentration source of this element in everyday life. The restriction on P is much less severe, because its all around. But really I dont see the point in restricting either, once you remove the ephedrine, the illegal use is gone, and they become ordinary chemicals. I wish theyd make chemistry a mandatory subject at school so all these lawyers and politicians would know what they are talking about.

Thanks Starman. I tracked down the PDF doc for the restricted poisons and drugs act in Queensland but that doesn't even mention iodine in its elemental form let alone KI. I'm not after I2 and have no intent on manufacturing any illegal substance so I guess I'll test the customs detection methods and see what happens. I will post the outcome if I'm able to

huh