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

Prepuce

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Re: Iodine & Iodine Crystals
« Reply #20 on: July 02, 2010, 04:47:42 AM »
Vesp, I started out at a low temperature--quite low, in fact, well under the boiling point of water. I didn't use a thermometer, though, so I can't give you a figure. But right away the moisture started coming off, before any I2 vapors. I should add that after the low temperature attempt I left the rig assembled overnight, and when I came back to it the H2SO4 had re-absorbed most of the moisture. However, it still held most of the I2.

The other thing that was strange was the way the H2SO4 held on to the I2. Eventually the heat was turned way up, but it didn't help. Maybe something out of the ordinary was going on, but if so it was nothing that was obvious.

I expected that the H2SO4 would have really held on to the water, not the I2, and would have bet money that the technique would work well.  That doesn't seem to be the case, and I'm guessing that this is one of those legendary methods that gets mentioned from time to time, but that on one ever really tried.

PP
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Vesp

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Re: Iodine & Iodine Crystals
« Reply #21 on: July 02, 2010, 08:10:00 AM »
Interesting -- was it pure H2SO4, or was it drain cleaner type?
How wet was the iodine and how much H2SO4? It is sounding to me that you didn't add dry enough iodine to enough dry sulfuric acid, or something strange was in it that trapped it -- I.e if the organic stuff in the drain cleaner was reacting with it, etc..


An idea is use a solvent that is similar to chloroform but doesn't react with the iodine and has a low boiling point, and extract it that way, perhaps? small amount of water would dissolve, Not to sure what would work in that situation, but I'd bet something could be found? hexane? no clue what would dissolve it, I know chloroform dissolves both chlorine and bromine really well, but begins to react with bromine, so it will react with I2 even faster.

Perhaps also with the solvent idea, it may not even need to dissolve the iodine, just form an azeotrope with the water, and use a dean stark apparatus - any of the iodine that sublimated in the condenser could than be scraped off, while hopefully leaving a good portion of it in the flask, and not much in the trap.
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no1uno

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Re: Iodine & Iodine Crystals
« Reply #22 on: July 02, 2010, 10:18:46 AM »
I would NOT USE EBAY!!! I PERSONALLY have been raided as a result of international purchases off ebay, which was resolved after a great deal of heartache and pain, but not before I lost some $10K worth of glassware/chemicals/equipment.

Feel free not to learn from my mistakes if you must, just realise they ARE watching.
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Re: Iodine & Iodine Crystals
« Reply #23 on: July 02, 2010, 11:18:18 AM »
Thanks for the warning.  That cat is out of the bag.  It wasn't an international order or very big one, just for experimentation.  At any rate the product appears as advertised, but haven't tried doing anything with it.  It is used in a lot of analytical chemistry reagents and I'm trying to learn to test my herbal extractions for various substances.  Safety!

I did USFSE on ebay busts before we started buying chemistry stuff there because I didn't want to get any trouble - you can get busted for having a still in this Podunk County.  There are certain things which seem to raise red flags and since people can review your purchases via your feedback rating, I assume whatever I buy is public record.

salat
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Prepuce

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Re: Iodine & Iodine Crystals
« Reply #24 on: July 04, 2010, 11:07:14 PM »
Ebay is notorious for LE sting operations. If you've ordered I2 from someone there it might be wise to prepare for a visit from someone who wants to ask you some questions about it.

Vesp, I2 dissolves in every organic solvent I've ever tried, and reacts with most. The best way to get it dry of which I'm aware is to squeeze it out in the filter as best as possible, then fold the filter up in paper towels and stand on it, then wrap it in a rag, place it between two pieces of plywood and squeeze it in a vice for 15-20 minutes.  After that it will be ready to re-sublime.

If you don't have a vice you can put it in an oversized glass or porcelain container, into which is inserted a smaller container holding dried epsoms or the like. The large container is covered but the smaller is left open. After a day or two the I2 will be very dry and ready to re-sublime.

PP
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« Last Edit: July 05, 2010, 01:26:32 AM by Prepuce »
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salat

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Re: Iodine & Iodine Crystals
« Reply #25 on: July 05, 2010, 03:42:38 AM »
I am always prepared to explain ad naseum what I intend to do with something, hard to shut me up!!

Iodine is all kinds of useful for making test solutions - at Least I read somewhere it was or was that iodate?

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Vesp

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Re: Iodine & Iodine Crystals
« Reply #26 on: July 05, 2010, 06:03:16 AM »
Iodine solution is used to test for the presence of starch, it turns a very dark purple or blue color. Of course, it also has other legitimate uses, such as sterilization, etc.

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Prepuce

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Re: Iodine & Iodine Crystals
« Reply #27 on: July 08, 2010, 02:20:26 PM »
It's also widely used as a tissue stain in biology. Such a versatile element--too bad it's difficult to procure these days.

PP
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DaMoose

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Re: Iodine & Iodine Crystals
« Reply #28 on: July 10, 2010, 12:40:00 AM »
Moose hasn't done ebay iodine since early 2000's

Just not kool unless you know of the seller from sombody..
maybe

it's just much simpler to get:

Triodine 7 Tincture - 16 oz.
Strong 2% Iodine available in a Topical Wound Dressing - superior for treating chronic inflammatory conditions and the control of ringworm, etc.

Regular Price: $7.99
Club Price: $7.11


from a long established veterinary supplier !

They used to sell 7% Tincture 16 ounce bottles for 12 bucks
Puking out like 48 grams of I !

Now the product has changed !
But it is still a stable source and safe.
16 to 17 grams for 8 bucks a bottle.
« Last Edit: July 14, 2010, 12:17:38 AM by DaMoose »

salat

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Re: Iodine & Iodine Crystals
« Reply #29 on: July 10, 2010, 01:25:48 AM »
I am always prepared to explain ad naseum what I intend to do with something, hard to shut me up!!

Iodine is all kinds of useful for making test solutions - at Least I read somewhere it was or was that iodate?

salat

Actually that was a bit of my dumb blond routine... I am intending to use it for testing - found a bunch of tests in some old pharmacy textbooks that I'd like to experiment with.
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iknowjt

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Re: Iodine & Iodine Crystals
« Reply #30 on: July 12, 2010, 09:43:17 AM »
It's used in forensics to immediately make fingerprints appear.....

There's a colorless iodide tincture, many drug stores around here have it right next to the normal 30ml bottles of purple tincture.

Quote
Active Ingredients:
Alcohol 45%, denatured with ammonia,
Ammonium and Potassium Iodides........Antiseptic

Two points worth noting about it:

 -Turns out you can pull 4.5g of elemental I2 out of one of these 5$ bottles.  That almost thrice the better deal.

 -Some of you might find this to be comical, but I was being sloppy using HCl and H2O2, and had re-titrated it back over with NaOH and then used HCl again to compensate.
I didn't think much of it when the crystals appeared to have a slightly reddish tint to them.
When i picked up the coffee filter they where drying in, a bit later, you should have seen the look on my face when suddenly it had exploded in my hands, leaving me temporarily deaf from the loud pop.
For some time after, little bits that where too small to see with the naked eye, would detonate from walking around the area.

Sometime later I stumbled upon the realization that I had made NI3, simply by having ammonia and elemental iodine in water.

This was my first ever experience with an energetic material.  There was clearly no real danger, but not knowing what was going on it was scary!  Now funny.



Dongle

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Re: Iodine & Iodine Crystals
« Reply #31 on: July 18, 2010, 03:13:52 AM »
Hah. The plumes of purple smoke must have been the grand finale!

Vesp

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Re: Iodine & Iodine Crystals
« Reply #32 on: July 18, 2010, 08:45:17 PM »
Quote
A few days ago, SWIM had a brainwave, after reading that DCM is one of the best solvents for iodine.

SWIM had a plastic bucket in which he had made some iodine out of KI / HCl / hydrogen peroxide. He poured it through some coffee filters in a big funnel, and ended up with the usual gooey mess of wet iodine, contaminated with peroxide, acid, potassium salts etc

He really hates making iodine, and wasn't looking forward to all the steps he usually takes to get the iodine clean and dry:-

THE OLD METHOD

wash the filter with cold water to remove some contaminants
lift the filter out of the funnel without it tearing
Squeeze excess water out with gloved hands
step on it to remove more water
Place it between the pages of a yellow phone directory, and place a weight on it
wait for a day
Hope that it's dry enough to resublime (in a pyrex jug on a hotplate, with a bowl of icewater covering the neck of the jug as a cold surface
Recover maybe 50% of the iodine as crystals, with the other 50% forming a rock hard contaminated mat in the base of the jug

What a pain in the ass.

Remembering his container of DCM, he tried this instead:-

THE NEW METHOD

Pour DCM through the filter of raw iodine, into a separating funnel
the iodine dissolved in a surprisingly small amount of DCM, giving a dark purple liquid in the separating funnel.. Lots of crap, hairs, and a dead fly were left on the filter paper
Top the separating funnel up with cold water, and shake the hell out of it
Two layers quickly separate out. The purple iodine stays in the lower DCM layer, whilst the contaminants  stay in the upper aqueous layer
Open the stopcock, and decant the iodine-containing DCM into a pyrex dish. Throw the water layer down the drain.
Allow the DCM to evaporate off outside. This doesn't take long, as DCM boils at 40C.

SWIM was left with a dish of concentric rings of clean iodine crystals, and a lattice of the longest iodine crystals he has ever seen in the middle.

Another interesting thing that SWIM found was that DCM with iodine dissolved in it can be boiled on a hotplate on it's lowest setting. He expected clouds of purple iodine vapour to come off with the boiling DCM, but this doesn't happen. Iodine is volatile, but not as volatile as dichloromethane, and it's so soluble in DCM that it wants to stay in the boiling solution until it's super-saturated. When this point is reached, an occasional wisp of purple vapour can be seen coming off. Remember, the boiling liquid is only the temperature of a cup of warm coffee.

SWIM assumes that this saturated DCM can be covered in clingfilm and placed in the freezer to crash iodine crystals out, but he hasn't tried this yet - besides, the remaining DCM will evaporate naturally within 30 minutes at room temperature.

I really recommend DCM to my fellow bees. Google it, and you will see how cheap and easy it is to get hold of. It makes it so easy to get dry, clean iodine in high yield.
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Prepuce

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Re: Iodine & Iodine Crystals
« Reply #33 on: July 26, 2010, 06:21:02 AM »
Is there an OTC source of DCM? I know you can buy it from chemical companies, but have never been able to find it in a store.

PP
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Re: Iodine & Iodine Crystals
« Reply #34 on: July 26, 2010, 06:35:48 AM »
Is there an OTC source of DCM? I know you can buy it from chemical companies, but have never been able to find it in a store.

you can distill it from paint stripper and brush softener. but some of the paint stripper sucks cause it has waxes and shit in it. the brush softener doesnt... its methanol, DCM, naptha. as you probably know, the naptha is over 100c and the methanol is 65c, so they can be left in the flask and discarded after you catch what comes over at 39-40c.

Prepuce

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Re: Iodine & Iodine Crystals
« Reply #35 on: August 02, 2010, 03:20:02 AM »
Thanks once again, JB. It looks like distillation is becoming ever more important.

It was noted today that silicone spray contains a large percentage of heptane. Not sure how easy it would be to distill, but heptane is another solvent you don't see every day.

PP
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Vesp

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Re: Iodine & Iodine Crystals
« Reply #36 on: August 02, 2010, 08:59:56 PM »
I believe heptane is also -- or pentane? is found in a high percent in a lot of spray on shoes sealers for leather, but I could be mistaken - it is some spray used for leather shoes. It is either heptane, pentane, or one of the *tanes that is a small and a liquid at room temperature.
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Re: Iodine & Iodine Crystals
« Reply #37 on: August 03, 2010, 03:27:42 AM »
Given that people are slinging around excess reagents and the like, anyone care to provide a stoichiometric equation? If, say, a pint of 16% iodine were used. How much H202 and HCl would ensure a full extraction of the iodine to elemental form? I'd like to know why this procedure works!

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.

Oerlikon

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Re: Iodine & Iodine Crystals
« Reply #38 on: August 04, 2010, 09:53:17 PM »
I never understood why people use these dirty and slow methods when you can get I2 fast simple and without much stoichiometri with KI(NaI)/HCl/H2O2.

Just dissolve KI/NaI in water,little as possible at room temp.,
ad same volume of conc. HCl
You will see some NaCl perticipated at the bottom.
You can decant them if you want.
Now add 5 times as much 3% H2O2
(for example,if you added 2ml of water and 2ml of HCl add 20ml of 3% H2O2),
swirl it a bit and filter the iodine,wash it with a little dH2O.

Crush it,mix it with some dry MgSO4 and resublime.
Hairs,dead flies and table slat won't sublime,unless you heat it way too much ;D
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