mr_pyrex (Head Coach)
03-08-04 07:31
No 493757
      Extraction of I from KI , Rhodium     

What I am looking for is the information that I have seen in the past on Rhodiums site, but now seems to elude me.  I have checked the site twice and have been unable to locate it, yes it is probably operator error (mr_pyrex's fault) but nonetheless it would be greatly appreciated if someone could post a link to it or even a extraction method that works for extracting I2 from KI.  Again thanks in advance.  Pyrex out of extraction techniques

Yeah and if ya don't PAID me well, I won't INFORMANT you of the answers you are seeking ;-)
 
 
 
 
    ApprenticeCook
(Newbee)
03-08-04 07:50
No 493760
      Pretty sure you could use the problem in the...     

Pretty sure you could use the problem in the production of HI for Iodosafrole to your advantage here, concentrated aqueous KI and drop in concentrated H2SO4 to make HI but then in water it is then turned into I2 by the oxidising radical left over from the acid isn’t that right?
This problem was solved in halo safrole threads by using DMSO instead of water but here seeing as you want I2 you could use this?? Dont know how successful it is though.

Any comments? Just a thought.
-ApprenticeCook
 
 
 
 
    Scottydog
(Hive Addict)
03-08-04 12:46
No 493800
      Felon     

Swim remembered reading this post in TSE and has yet to confirm its accuracy. Has been meaning to dream this up for quite some time.

Post 405764 (felon: "experience with this method", Stimulants)

Has any one else attempted this? Its been buried at the bottom of Swim's bookmark section, for what seems like forever. crazy

Could probably get by on half the amount of muriatic acid?

Was always curious as to what percentage of hydrogen peroxide he was using as well. Geez mentions using 1 bottle of 3% hydrogen peroxide on one pint of 7% tincture, so surely "Felon" was referring to the 30%+ beauty store variety?

Will someone once and for all set this straight?

KI is soooo fucking cheap and easy; ordering I2 is soooo fucking risky. frown

Please share the wealth, God only knows that Swim has recently.

PM if necessary...

Thanks bees.

Refuse/Resist
 
 
 
 
    SHORTY
(Hive Addict)
03-08-04 14:16
No 493811
      I asked the same question a long time ago...     

As far as i can remember, the best results were achieved when the KI was dissolved in dh20 to make a 10% solution and then adding hcl and h2o2.  The problem is i never did work out the ratios.  I do remember that if the solution is more than 10% it will get really hot when adding the h2o2.  However, i was using 18% h2o2. 

I too would like to see what the correct ratios are suppose to be. 

Here are some links to my past quiries on the suhject.

Post 414524 (SHORTY: "How bout a little advice?", Stimulants)
Post 404797 (SHORTY: "Potassium Iodide + H2O2 too hot too handle!", Stimulants)
Post 109151 (Osmium: "Home-made I2", Stimulants)

It wasn't Me!
 
 
 
 
    quantum
03-08-04 18:44
      ill try the h202 and hcl
(Rated as: insignificant)
    
 
 
 
    mr_pyrex
(Head Coach)
03-08-04 20:16
No 493858
      Well let me thank you all for all of your very     

Well let me thank you all for all of your very helpful insights and I will be sure and repay you all by locating all the available info pertaining to this type extraction and as soon as I get some extra time to experiment with any of the varibles I will post a write-up with all the details needed for successfully extracting I2 from KI.  Again THX.  Pyrex out of time at the moment ;-)

Yeah and if ya don't PAID me well, I won't INFORMANT you of the answers you are seeking ;-)
 
 
 
 
    mr_pyrex
(Head Coach)
03-08-04 20:34
No 493860
      Here is some information that I did have from...     

Here is some information that I did have from Worlock's website back when it was available...I am uncertain as to who the credit goes to since it doesn't say within the post.  It isn't directly related to I2 extraction from KI but maybe it might bee of some use to someone.  Pyrex out of archived info :-)





Converting iodine tincture
Tincture of iodine is iodide salts in alcohol, it is found in supermarkets in small one ounce bottles. Each bottle can generate a little over a gram of I2 the price has shot up from 0 .60 cents to $1.80 / bottle. Tincture comes in 2% or 7%. XXXX XXXX carrys 2% for $.87.
It is also available at feed and tack stores in pints and gallons.

Formula one
1 pint 7% tincture iodine
3 pints of hydrogen peroxide
2 oz of HCl
1/2 cup of d-H20

Shake it up, in a one gallon jug,
Wait 20 minutes
Filter through a pantyhose
Wring out fluids.
Put iodine crystals in a glass jar,
Re-wash four times with distilled water, cover, shake, pour off the water into a filter
On the final water wash, wash the iodine into a into a fresh filter,
Wring it out hard,
Open up filter roll into a dry filter
Wring out hard
Put crystals in a dark place to dry.
Use a Drying agent like Calcium Chloride store with the I2 in a sealed chamber
Grocery stores, for mildew prevention near the moth balls
I2 is light sensitive and will degrade.
When completely dry store in light resistant container..
Formula 2
1) 1000 ml 2% Iodine tincture = 2.5%I+2.5%KI in etOH and H2O =-
2) 250 ml Muriatic acid = 34.4%HCl
3) 475 ml Hydrogen peroxide = 3% solution of H2O2
4) 1750ml Distilled H2O
In a 1 gallon container (plastic or glass),
mix 1 liter of 2% tincture of iodine
with 250 ml of Muriatic acid
stir and allow to sit for 15 min.
Add 475ml of a 3% hydrogen peroxide
stir and let sit an additional 15 min.
Add 1750 ml distilled H2O
shake and let sit for 15 min more.
An orange water layer appears on top of a dark gray layer of I2.
Pour off most of the the orange water
Add fresh distilled H2O shake and let sit
Pour off most of the the orange water
Wash a total of three times with distilled water (more can't hurt)
On the last wash pour the I2 into a stack of 5 coffee filters
Wring it dry
roll the iodine ball into 5 dry coffee filters
Wring it dry
Roll it into 5 more dry filters
wring it dry
Put the I2 in a small clean glass jar break up the iodine ball
place the jar of I2 on a piece of cardboard, cover the I2 with a larger jar
put in freezer for several hours
Remove jar of I2, seal it tight, with cellophane then screw on the cap store it in a dark cool environment
Potential problems Not rinsing the I2 enough with water to remove the chlorine and salts from the tincture Not drying the I2 out enough and adding it too wet to your reaction. If in doubt at all re-wash the iodine with distilled water in a filter and wring out, The iodine is only very slightly soluble in water, you lose very little washing with water. If it is not clean and dry you can lose a lot more in a failed reaction.
And yes both of the above methods do indeed work as is.. I have used both personally.  Pyrex out

Yeah and if ya don't PAID me well, I won't INFORMANT you of the answers you are seeking ;-)
 
 
 
 
    Scottydog
(Hive Addict)
03-09-04 05:49
No 493943
      Thanks Shorty and Pyrex     

According to Geez, 3 bottles of h2o2 is overkill for the 7% tincture recipe.

Swim might just take the KI and line up a bunch of 1 pint bottles. Then dilute the KI into a huge volume of 7% solution. (thanks Shorty)

Fill up the pint bottles and then run each of the pint bottles through its own individual extraction with Geez' info found here:

Post 311336 (geezmeister: "I2 from tincture", Stimulants)

I guess it would probably bee better to break up the lot of KI into these smaller extractions then to run a bulk extraction per Felon.

Kind of like nanos, that way if Swim fucks up while dreaming , he will only lose a little bit, rather then all at once.

Might make for the cheapest I2 yet!

Now the only thing Swim has to determine next, is what percentage of yield one might expect from the conversion. wink

Thanks for bringing up this once buried discussion. cool

Refuse/Resist
 
 
 
 
    SHORTY
(Hive Addict)
03-09-04 12:43
No 494017
      Well i beleive the yeild was....     

70g of iodine from a 100g bottle of KI.  That was carried out in a similar way that you are considering.  Its easier to work with in smaller more diluted solutions and i think if you do it the way you propose you will be quite happy with the results.

Where i live it is harder to get KI than it is iodine and its the same price!  However, when i do get KI, i prefer to use phosphoric acid and make HI rather than making iodine.  Its actually easier to do it that way in my opinion but thats just an opinion. 

Look forward to hearing your results SD and that writeup Pyrex!

It wasn't Me!
 
 
 
 
    SHORTY
(Hive Addict)
03-10-04 09:47
No 494227
      Well, i went ahead and tried it again..     

I used a 100g bottle of KI which i added to a 2.5 liter chemical bottle along with 1100ml of dh2o and then added approximately 50ml of 37%HCL and shook and then added about 75ml of 18% H2o2 and shook and instantly had a layer of iodine crystals about 4 inches thick sitting on top of the solution.  The bottle was warm but not hot like before.  Anyways, i filtered out the crystals and when they dry i will post the weight.  Im guessing around 70g by the looks of it.

It wasn't Me!
 
 
 
 
    mr_pyrex
(Head Coach)
03-10-04 20:53
No 494312
      Shorty-You mentioned that you'd rather use...     

Shorty-You mentioned that you'd rather use phosphoric(sp?) and make HI...I vaguely remember reading something recently here about that I think, anyways once you make the HI which type rxn are you using it in??  If I might ask...not being sarcastic...just thinking maybe I might be able to improve on the route using now...which is dry push/pull with red p.  The finished product is quite good, however I know it could be better...a person from the past had proven this to me...only problem is that he ended up taking a extended vacation before I could sit in on a run or even get the specifics on how he was able to go from 'good' to 'PERFECT' almost overnight.  Anyhow...any insight would be greatly appreciated and let me again say thanks to all those fellow bees who have taken the time to contribute to this thread.  Pyrex out of time at the moment ;-)

Yeah and if ya don't PAID me well, I won't INFORMANT you of the answers you are seeking ;-)
 
 
 
 
    shinymetallic
(Stranger)
03-11-04 16:14
No 494503
      KI Tablets     

This newbee can find the KI tablets all over the place but the KI solution they find is usually only 1%.  Could this newbee use the tablets dissolved in dh20 to make this solution?  Is this the technique you used Shorty?  Another (I hope) not too dumb question.  How would this newbee determine the % of the solution if the tablets and dh2o were used?  Thanks.
 
 
 
 
    ApprenticeCook
(Hive Bee)
03-11-04 18:33
No 494531
      Tablets     

As long as the tablets only contain KI with no other stuff in it. Check the packet.

If you’re using tablets as in the kind which you buy to treat your thyroid the actual KI content will be low in each tablet leading to more packing to be used, be careful as you would need to sperate out the KI content from the packing, check the packet for contents of each tablet.

To work out % w/v of a solution (for a solid dissolved in dH2O) take the number of grams of solid (KI) and divide it by the number of mL's of water you add to dissolve it, multiply that number by 100 to get your concentration in %w/v.

-ApprenticeCook
 
 
 
 
    SHORTY
(Hive Addict)
03-11-04 19:14
No 494543
      Hypo     

The HI obtained from KI and phosphoric acid was used along with hypo to do the rxn.  However, i beleive rp would work just as good but will take a little longer.

After this latest result of KI to I2, I might reconsider making HI due to the slightly more complicated process.  I have only tried the conversion a few times and previous attempts were rather frustrating and time consuming.  However, this last attempt took less than 10 minutes and was only a matter of adding, shake, adding, shake, filter, wash, dry. I still can't beleive it was that easy.

It wasn't Me!
 
 
 
 
    mr_pyrex
(Head Coach)
03-12-04 03:04
No 494595
      So shorty it sounds like your mixing KI and...     

So shorty it sounds like your mixing KI and H3P04 and then from this mixture you'd get HI and Potassium Phosphate...Is this correct?  And if so, they don't just go together and then like magic you have HI once you separate out the potassium phosphate do they??  Mind you I am NOT being derogatory in any way...I am just trying to figure out if I am understanding the process correctly and what the process would theoretically yield.  Well I think  I will also review some of your recent posts and maybe in the process of reviewing posts...I'll be able to answer these questions myself :-)   Pyrex out using search engine ;-)

Yeah and if ya don't PAID me well, I won't INFORMANT you of the answers you are seeking ;-)
 
 
 
 
    SHORTY
(Hive Addict)
03-12-04 05:14
No 494618
      Well its not quite that simple     

The procedure involves distilling the phosphoric and KI at high temperatures.  The distillate is the HI.  Heres a few links:
 Post 438386 (SHORTY: "Hi from KI", Stimulants)
Post 446436 (SHORTY: "Trying the above HI preparation procedure", Stimulants)

It wasn't Me!