Author Topic: Iodine & Iodine Crystals  (Read 608 times)

llamabox

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Iodine & Iodine Crystals
« on: March 02, 2009, 02:19:14 AM »
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« Last Edit: June 30, 2010, 05:54:35 AM by Vesp »

Vesp

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Re: Iodine & Iodine Crystals
« Reply #1 on: March 02, 2009, 02:25:12 AM »
Iodine can also be made from the Iodine tincture that can be obtained at most stores for a pretty high price.
This can be done by bubbling chlorine into the solution which will precipitate small iodine crystals.
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llamabox

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Re: Iodine & Iodine Crystals
« Reply #2 on: March 02, 2009, 02:29:12 AM »
So this bottle of 2% (USP) Iodine tincture in my first aid kit.
It says... 2% Iodine, 47% alcohol, Sodium Iodine 2.4% and purified water.

Vesp

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Re: Iodine & Iodine Crystals
« Reply #3 on: March 15, 2009, 07:42:45 PM »
Sweet.. going to get some I2 crystals from it?
Is it just one of those small 1oz bottles?
I've heard rumor they are going to change the scheduling on iodine substances, including the tincture.
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LYC

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Re: Iodine & Iodine Crystals
« Reply #4 on: March 15, 2009, 08:14:38 PM »
Its nice to see a source for the I2 crystals, thanks Lamabox! The Providone iodine stuff I got is a total is a pain in the ass, I wish there were a way to easily extract that stuff. I've seen the methods but its always way more work then I'd like to spend on it.

Vesp

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Re: Iodine & Iodine Crystals
« Reply #5 on: March 15, 2009, 08:21:39 PM »
Yeah.. but the best method is probably just to use potassium or sodium iodide and bubble chlorine gas into that, which will lead to I2 being precipitated out. Then you can take the I2, add H2SO4 and sublimate to get some nice dry I2 crystals.  the main drawback is that you are going to have to buy the KI offline from some chemical vendor, but really that's not much of a big deal at all.

Edit: You could also just react the KI with an oxidizing acid (sulfuric, or nitric?) and then you don't have to mess with the chlorine.

Here is a video on how to make Iodine from KI and H2O2: http://www.youtube.com/watch?v=CLhwkFKLdPA&feature=related
I don't think that is a very good method since the solution would probably get pretty dilute using 3% H2O2, and if you didn't react all of the KI the I2's solubility would increase dramatically.
« Last Edit: March 15, 2009, 08:28:25 PM by Vesp »
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xxx

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Re: Iodine & Iodine Crystals
« Reply #6 on: March 16, 2009, 06:16:57 PM »
Here is my method for making I2 crystals:

Place 10cc dilute H2SO4 and 1 gram KI in a conical flask.
To this add 25cc of Bleach (5.5% NaOCl soln. in my methods)

The I2 should ppt out and is easily vaccum filtered or whatever, then sublime to purify.

Its honestly that easy!

Vesp

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Re: Iodine & Iodine Crystals
« Reply #7 on: March 17, 2009, 12:24:30 AM »
Oh yeah, I knew there was another easy method.
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llamabox

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Re: Iodine & Iodine Crystals
« Reply #8 on: March 23, 2009, 05:46:14 PM »
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« Last Edit: June 30, 2010, 05:54:14 AM by Vesp »

Vesp

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Re: Iodine & Iodine Crystals
« Reply #9 on: March 23, 2009, 11:21:04 PM »
That looks like a pretty good deal -- little bit more then I like to pay for chemicals but that is pretty cheap or iodine crystals.
Since Iodine is so easy to make from iodides, know any cheap sources of say potassium iodide?
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llamabox

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Re: Iodine & Iodine Crystals
« Reply #10 on: March 23, 2009, 11:58:51 PM »
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« Last Edit: June 30, 2010, 05:53:57 AM by Vesp »

poisoninthestain

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Re: Iodine & Iodine Crystals
« Reply #11 on: March 25, 2009, 07:02:34 AM »
in situ chlorination of the iodine ion...

calcium hypochlorite + h20 + any salt of iodine + (titration of con. HCl) -> I2 + metal salt +Cl2...

...plus some other miniscule side reactions. that's basically it.

You should use an excess of HCl until no more iodine precipitates. Simple as that.

Sedit

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Re: Iodine & Iodine Crystals
« Reply #12 on: April 17, 2009, 02:29:56 AM »
http://www.youtube.com/watch?v=2F_kPXbi2D8&feature=player_embedded

To cool not to share, Gives the whole process in time laps from KI or NaI thru sublimination.
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German

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Re: Iodine & Iodine Crystals
« Reply #13 on: August 03, 2009, 02:17:20 AM »
You can also get I2 crystals from seaweed. You can buy the seaweed I think at an aquarium or something like that, I forget.

heisenberg

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Re: Iodine & Iodine Crystals
« Reply #14 on: August 14, 2009, 09:37:56 PM »
The first source listed has a DEA reporting disclaimer at the end of the page.
« Last Edit: August 14, 2009, 09:44:25 PM by heisenberg »
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Prepuce

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Re: Iodine & Iodine Crystals
« Reply #15 on: June 30, 2010, 04:34:39 AM »
This is an old thread, but since the information is still here (and in other places as well) I thought one more response might  eventually be useful to someone.

When I read it I thought the idea of drying and re-subliming I2 at the same time by mixing it in H2SO4 was a really clever idea. I still think that, but here's a report on using the method.

About a gram of wet I2 was placed in a flask and a few mls. of concentrated H2SO4 were added. A condenser was fixed to the flask and the flask was heated. It was noted that the moisture in the I2 + H2SO4 mixture vaporized more readily than the I2, never the less the process was continued for about an hour at several heat settings. Regardless, the result was the same--wet, messy crystals condensing. In every case the water vapor rose higher than the I2. It was also noted that significant amount of the I2 did not sublime, but remained mixed with the H2SO4 in the flask regardless of the heat settings used.

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Vesp

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Re: Iodine & Iodine Crystals
« Reply #16 on: June 30, 2010, 05:52:04 AM »
Don't heat it as much -- if it gets to hot, the H2SO4 will lose water, however, it is kept cooler, it should keep it fairly well, just make sure to add an excess amount of H2SO4 so there isn't much water.

I haven't ever done this, but I assume one of the problems (though, there could be many and this method may not work) is that you are simply heating it to high, and not making it into the zone where the water still is kept from leaving because of the H2SO4, and where the iodine sublimates at a decent rate.

How hot would you say you got it?

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drone1240

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Re: Iodine & Iodine Crystals
« Reply #17 on: June 30, 2010, 06:30:19 PM »
The benchmark of this group is so high I seldom get to add anything useful but the thought of you fellas toying with chlorine gas makes me glad to take a few minutes and tell ya what I did back when I had a reason to need I2:

1 pint 7% Iodine tincture
3 pints H2O2
4 ounces 30%HCL

Mix the said in a gallon milk jug. Let it sit for a spell than shake again. Pour contents into another milk jug with a funnel and a piece of panty hose. Most of silvery elemental I2 at bottom of jug. Nitrile gloves are a good idea at this point. Wash contents inside panty hose with some dH20 to wash off residual HCL than transfer to a stack of 10 coffee filters and ring out. Open coffee filters and cafefully take the first one or two out of the other 8 and put in ten more. Ring hard again to take out more water and put them in a pill bottle or what ever. Most of the water should wick out into other filters. Sublimate if necessary.  16oz x7% =1.12oz I used to get it by the gallon for 28 bucks. 128 x .07 = 8.96 ounces for 28 bucks. Just gotta put your overalls and straw hat on. Them feed store folk weren't as hip back then as they are now but its still there.

Edit. I dont know why peroxide and HCL drop the elemental I2 out of solution but the do. You dont have to be exact on how much HCL you use. I didn't measure the stuff towards the end of me making it and my yields were always  near perfect. I could go from a bottle of tincture to a ball of crystals in a filter in less than a half hour.
« Last Edit: June 30, 2010, 06:41:51 PM by drone1240 »
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salat

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Re: Iodine & Iodine Crystals
« Reply #18 on: July 01, 2010, 11:43:48 AM »
You can buy it at ebay - at least one seller from Indiana had decent prices for crystals.  Also sometimes you can find it in vintage medicine bottles section.  Most of the metallic elements seem to hold up pretty well.
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Vesp

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Re: Iodine & Iodine Crystals
« Reply #19 on: July 01, 2010, 08:31:03 PM »
I have heard bad things about ordering from ebay.
SM has a lot of comments on it that may be worth reading.
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