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Author Topic:   Home-made I2
Osmium
Member
posted 05-27-98 02:09 AM     Click Here to See the Profile for Osmium     
This is just an idea, and I have no proof that it really works, but hey, go to the library and check it yerself.

First, obtain some NaI or KI. Dissolve it in water.
Second thing we need is a strong oxidising agent, like NOx (nitric acid + Fe wool), Cl2 (acidify bleach, or HCl and permanganate or MnO2), maybe even H2O2 or HNO3, which is bubbled through the iodide solution, or simply add one of the oxidisers to it. I don't know which one works, read and experiment.
This oxidises the iodide to iodine. Extract I2 with suitable solvent or distill I2 away with a stream of air to separate most of the inorganic shit.
Crude I2 is purified by sublimation. To do this, place crude I2 in a crystallizing dish and add some KI. Fill a large round-bottomed flask with cold water and place it onto the glass pot containing the crude I2. Now carefully heat the crude I2. It will evaporate and crystallize on the outside of the flask. Carefully remove it to obtain quite pure I2.

Osmium
Member
posted 05-27-98 02:31 PM     Click Here to See the Profile for Osmium     
Nobody interested?

O. checked it himself. It can be done, of course.
Oxidising agents like H2O2 in dil. HCl, Cl2, nitrite/H+, oxygen with NOx catalysis, K2Cr2O7, KMnO4, MnO2, bleach or PbO2(all in acidic soln) can be used.
The iodine is separated from the reaction mixture by (steam) distillation. Solubility of I2 in H2O is low (0.8g/l), all the crystals can be filtered away. Dry them in a desiccator over conc. H2SO4 or CaCl2 and purify by sublimation. Heat with sand bath. To avoid other halogenides as contaminants, especially when using Cl2 or bleach as oxidiser, grind the raw iodine with powdered KI before subliming.

Voila, OTC iodine, in huge amounts and inexpensive

Tlange
Junior Member
posted 05-27-98 05:52 PM     Click Here to See the Profile for Tlange     
Brilliant....now if the RP was only as easy to make...hmmm. ;-)

Osmium
Member
posted 05-28-98 02:52 AM     Click Here to See the Profile for Osmium     
I'm working on it ;-)

Osmium
Member
posted 07-01-98 04:41 AM     Click Here to See the Profile for Osmium     
Hope you'll find it now, jimwig.

jimwig
Member
posted 09-30-98 05:42 PM     Click Here to See the Profile for jimwig     
Osmium - I have finally found it after almost ten months of searching all over the globe via the net of course. I can finally quit and take a shower- thank God!!!!!

drone 342
Member
posted 10-15-98 10:08 AM     Click Here to See the Profile for drone 342     
Os,

Do you have a work-up method for this now?

-drone #342

300 Spartans
Junior Member
posted 10-17-98 05:20 AM     Click Here to See the Profile for 300 Spartans     
try gathering the mushing into a pulp pacific kelp boil the shit out of it till dry then add you oxidizer and acids aka osium let steep filter then heat placeing a round fish bowl over the top of your containerand as the man said Presto! unlimited and cheap supply of iodone crystals

Osmium
Member
posted 10-17-98 10:13 PM     Click Here to See the Profile for Osmium     
Drone: As I said, solubility of I2 in water is low, as long as no excess of I(-) is around. Simply filter it away or extract with organic solvent.
For bromine I recommend distillation of the reaction, or maybe blowing air through the solution and collecting it in a cold trap. In situ preparation of Br2 is probably best for brominations. I don't think extraction of Br2 is a good idea (cough, cough...). Reagent grade KBr from Merck is on its way to my house, and I will try it when I find the time.

drone 342
Member
posted 10-20-98 01:10 PM     Click Here to See the Profile for drone 342     
Os,

The extracting works pretty well for Br2 -- just use toluene. The toluene bromine solution is fractionally distilled (with an aspirator), and pure bromine is aquired. The advatntage is that by extracting with a solvent, you can get the volume of for your starting material for your distillation down, but the purity of the final product up. Nothing to it, though I'm definately interested if you have a better method. I look forward to labnotes.

-drone #342

HoneyDream
Junior Member
posted 07-20-99 11:58 PM     Click Here to See the Profile for HoneyDream     
Where can i obtain some I2? sorry to sound lame, but if i have a question and i cant find it on search, or anywhere else the best i can do is ask.. what exactly is I2, iodine crystals?

pebble
Member
posted 07-21-99 12:54 AM     Click Here to See the Profile for pebble     
I know that there are different ways to make iodine crystals and everybody it seems, has their own way. I have found that this works for me and it's quite easy to do. Here is the synth for making iodine crystal using tincture.

Get a one gallon jar. Pour in 16 1oz. tincture bottles that contain 2% iodine, this is two cups. Then pour in a cup of muratic acid. The add two cups of hydrogen peroxide and then a cup of 70% ribbing alcohol. Shake this up and let it sit for 5 min. Then come back and fill the entire jar with very cold DH2O. Cap it and let it stand for 20 min. (Do not shake this time).

Then get a couple of coffee filters and filter the liquid along with the iodine crystals. Then pour a little cold DH2O to stablize contents and taks your filters and squeeze out all water and then put your iodine crystal in a jar and you'll pure iodine crystals. It's really that easy. Other methods are also similar and others are just hard and complicated and a bullcarp waste of time. Try it and you'll see just how easy it really is.

Pebble

HoneyDream
Junior Member
posted 07-21-99 02:17 PM     Click Here to See the Profile for HoneyDream     
thank you pebble. one question about that:

At the end, you said filter the liquid in a
coffe filter, squeeze out the water from the
filters and you have pure iodine crystals.
my question is: are you saying the iodine
crystals will get stuck in the filter? as in
the liquids will go through the filter but
the iodine wont, and so all in your filter is
pure iodine crystals?

thankx.

pebble
Member
posted 07-21-99 03:37 PM     Click Here to See the Profile for pebble     
Yes, just filter and at the bottom of the jar will be the iodine. You'll see it when you pour all the contents out. It will look like mush until you squeeze out all of the water. When you squeeze out all of the water, you'll have iodine crystals that the filters contain. Dump these in a jar. These are also light sensitive, so keep them away from light.

Pebble

Soldier
Member
posted 07-21-99 06:06 PM     Click Here to See the Profile for Soldier     
A quick way to test the purity of the Iodine from these methods is, take a small amount of I2 (about the size of the head of a pin or a little larger), put in pyrex dish, and heat in some safe manner. The I2 will sublimate. If the residue left is granular in texture then IODIDES are still present which washing with DH2o should take care of.

------------------
A little revolution...is a good thing. Thomas Jefferson

CHEM GUY
Member
posted 07-24-99 04:48 PM     Click Here to See the Profile for CHEM GUY     
drone 342,

Last time I checked elemental halogens reacted with unsaturated carbon bonds with or without light present.

Br2 + C6H5-CH3 --> C6H5Br2-CH3

Merry Crankster
Junior Member
posted 07-28-99 09:52 AM     Click Here to See the Profile for Merry Crankster     
while dreaming anothers dream I screwed up but the results were exellent, heres how it whent.

Dreamer misread h2o2 (hydrogen peroxide right) as dh2o(distilled water, right).

1 pint 7% tincture iodine(from feed store)

added to this 3 pints dh20

+ 1/2 cup of muriatic acid(hardwarestore stuff cement cleaner)

then said oops that should have been h2o2 insted of dh20.......

so then added 1 pint h202 nothing happening yet. so went to the hive and saw something about bleach and muriatic extraction of Iodine tincture.

so said what the hell and added bleach about 1/2 cup and whalla solution became clear brown color with lotso darke colored cystals floating around in there.

filtered crytals through a few coffee filters in funnels pressed out extra liquid and air dried an hour or so. Looks like killer Iodine grey purplish crystle flakes/granules.
dreamed it in Hi/rp reduction at 1 part to 1 part Pephedrine with 1/2 part rp good product 50-60% return.

outlaw
Member
posted 07-30-99 03:51 PM     Click Here to See the Profile for outlaw     
Ok I have a friend who has a plastic bag with
containing Organic iodine 40\salt base
ingrredients are ethylenediamine Dihydriodide,salt,artificial color, silicon Dioxide. Also says Salt(NaCI}minimum-87%
maximum-91%. can anyone give advice on what needs to be done to this for clean I2 if anythying. Believe me the search engine has been my life for over a month so if anyone can help Id apreciate it. Happy dreaming to all.

Demented Angel
Member
posted 11-21-1999 01:54 AM     Click Here to See the Profile for Demented Angel     
I know this is an old thread, but was wandering around the Hive, came across it, and thought, "Hey, since folks have posted a couple of quick and easy ways to get I2, and since 'How do I get I2?' is a commonly asked question, why dont I go ahead and post a method I came across?"

So here goes. I came across this method awhile ago, and dreamt that it worked very well.

This was originally posted by cantstanditanymore, and has been rewritten by me because I have misplaced the original document. Oops!

DA


Iodine Extraction
-----------------
Originally posted by cantstanditanymore

Ingredients:
1 pint tincture of iodine (7%)
3 pints hydrogen peroxide (3%)
1/2 cup distilled water
1/2 cup muriatic acid

Other things needed:
1 gallon jug
1 set rubber gloves - nothing says cook like iodine stained fingers!
coffee filters
more distilled water for rinsing of product

Put tincture, peroxide, acid, and distilled water in your clean gallon jug. (Note, as with all chem equipment, only clean it with distilled water.) Cap the jug and shake well. Set aside for 20 minutes or so. Go watch an episode of South Park while you wait. Pour off excess liquid. Take 2 coffee filters, placing one inside the other, and filter remaining product through the coffee filters. When filtration is complete, roll up product in filter and squeeze firmly to remove moisture. Transfer to clean set of coffee filters and rinse crystals with distilled water. Do this 4 times to clean your product. Once again, squeeze firmly to remove as much moisture as possible. Place product on clean, dry filters or in pyrex dish, and set in a dark place to dry. As soon as is dry, transfer product to dark, airtight container. Approximate yield, 16 grams.

Demented Angel
Member
posted 11-21-1999 03:21 AM     Click Here to See the Profile for Demented Angel     
Oh, one thing I nearly forgot. Original post told of using pantyhose to filter crystals out. In my dream I didn't have any hose around so used the coffee filters. Hose seem like might have worked easier.

DA

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