Author Topic: IODINE CRYSTALS FROM IODINE TINCTURE.  (Read 88 times)

llamabox

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IODINE CRYSTALS FROM IODINE TINCTURE.
« on: March 24, 2009, 12:08:18 AM »
DESCRIPTION

IODINE TINCTURE IS AN ALCOHOL BASED SOLUTION OF IODINE SALTS.  IT IS COMMONLY SOLD IN DRUGSTORES AS A OLD TOPICAL ANTISEPTIC.  AT TIMES, IT IS USEFUL TO HAVE CRYSTALLIZED IODINE, OR I2.  I2 CAN BE FOUND IN NUMEROUS PRODUCTS, HOWEVER EXTRACTION IS USUALLY DIFFICULT OR EXPENSIVE.  PURE I2 CAN BE USED TO DISINFECT SUSPICIOUS DRINKING WATER.  IT ALSO HAS USES IN EXPLOSIVES.

THIS SIMPLE PROCEDURE WILL CONVERT THE SALTS IN TINCTURE TO I2 WHICH WILL FALL OUT OF SOLUTION AS FINE PURPLE CRYSTALS.
 

MATERIALS       
-30% HYDROCHLORIC ACID - "MURIATIC ACID" IN HARDWARE STORES
-BLEACH
-TINCTURE OF IODINE
-COFFEE FILTERS

EQUIPMENT       
-MISC. GLASSWARE

1.  FIND SOME TINCTURE OF IODINE.  IT COMES IN SMALL BOTTLES AND IS SOMEWHAT EXPENSIVE.  YOU MAY HAVE TO SEARCH HARD BECAUSE ITS SOMEWHAT OBSOLETE NOW.  DO NOT USE POVIDONE IODINE.


 2.  POUR A FEW BOTTLES INTO A FLASK.

USE MORE THAN ONE BOTTLE AT A TIME.  THE REASON IS THAT YOU'LL LOSE A FRACTION OF THE IODINE IN VARIOUS WAYS, AND IF YOU USE A SINGLE BOTTLE THERE WILL BE TOO LITTLE IODINE LEFT TO RETRIEVE SUCCESSFULLY.

 3.  ADD AN EQUAL VOLUME OF WATER TO THE IODINE.  THEN ADD ABOUT ~5ML OF HYDROCHLORIC ACID PER BOTTLE OF IODINE.  STIR.  THEN ADD ~10ML OF BLEACH PER BOTTLE OF IODINE.  STIR.  BEWARE FUMES.  YOU SHOULD SEE THIS:

THE ACID HELPS CONVERT THE IODINE SALTS (KI, NaI) TO THE DESIRED FORM.  NOTE, EXCESS REAGENTS IS USUALLY NOT A PROBLEM.

 4.   PREPARE TO FILTER BY PUTTING TWO COFFEE FILTERS OVER THE MOUTH OF A BEAKER.

BE SURE TO USE TWO OR MORE FILTERS.  THE ACIDS WILL ATTACK THE PAPER, AND ALONG WITH MOISTURE, CAN BREAK THE FILTER.


 5.  DILUTE AND FILTER THE SOLUTION.  YOU NOW HAVE  I2.

Vesp

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #1 on: March 24, 2009, 01:27:58 AM »
Awesome! Great pictures, this is definitely going in the archives once I get the templates and everything set up better then it is now.

Are you planning on drying the iodine?
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llamabox

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #2 on: March 24, 2009, 01:32:51 AM »
Yea. The only things I have access to are MgSO4 and silica gel. So I hope on of them will work well.

Vesp

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #3 on: March 24, 2009, 01:36:19 AM »
Yeah, I'd try mixing anhydrous MgSO4 with the I2 and then sublimating it if you are able too.
You can also probably get some pretty ~92-95% sulfuric acid as drain cleaner at most places. You could mix the I2 with a few drops of that and then sublimate it.

Sublimation is kind of tricky for me, I left the I2 i got from a method fairly similiar to this one wet just because I didn't want to risk losing the I2.
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llamabox

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #4 on: March 24, 2009, 01:46:45 AM »
True. With it being wet would just reduce the amount of h20 needed for reaction later.

Vesp

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #5 on: March 24, 2009, 02:03:30 AM »
Yeah, but it just depends on what you are wanting to use it for. You can always dry it later of course :)
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llamabox

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #6 on: March 26, 2009, 03:54:03 PM »
The above TEK states, 5ML OF HYDROCHLORIC ACID PER BOTTLE OF IODINE.

Geezmeister at WD states, For one ounce bottles of tincture by the HCl/peroxide method, you should change your ratios significantly. One fl ounce of two percent tincture calls for about 0.75 ml of HCl acid at most. You could easily do with 0.5 ml of HCl acid. The excess, if not too great, will not hurt anything provided you rinse the excess out.

He also suggests using 3% Hydrogen Peroxide instead of bleach. Though with the same ratio. 10 ml per 1oz bottle of the iodine tincture.

Vesp

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Re: IODINE CRYSTALS FROM IODINE TINCTURE.
« Reply #7 on: March 26, 2009, 10:59:37 PM »
Yeah, considering the solubility of Iiodine by itself, and the fact that it can get kicked out of solution from the chlorides and other compounds, I doubt a few mL's is going to affect it to horribly. You  can get it cold to help any of the dissolved iodine fall out.
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