Hi everyone,

as always, I apologize if thi is being discussed somewhere else round here. Couldn't find.

Issue is:

I was dreaming of me having a hydroalcoholic solution of I and KI.


It is 50 ml containing:

- 3.5 g of I
- 2.5 g of KI

In the dream i didn't know about the alcohol ratio. So I figured I would just boil it out.

Then I dreamed I wondered If I could convert the KI in I via electrolisis.

Two bechers, one with the I/KI solution with the anode in it.
A saline bridge connecting this beaker to the second containing water with NaCL. And the Catode.


In my dream potassium was moved to the catode, passing in the second beaker. I- and Cl- moving to the anode, in the first glass. Cl2 thus formed flying away.

Would it work, in your dreams?

Thanks

If you can get bleach and hydrochloric acid, that's your best bet.

Boil off the ethanol. Add bleach, then hydrochloric acid SLOWLY.

NaOCl + 2HCl ---> NaCl + Cl2 + H2O

2KI + Cl2 ---> I2 + 2KCl

The iodine will precipitate.

If you are dreaming, you are better off on a different forum.

I used the NaOCl + HCl method with success. IMHO this is method with KI is so easy that it would be wasteful to try anything else. http://www.dererumomnis.org/bbs/index.php?topic=293.0

I read the thread you linked.

questions:

i read twice your post, enkidu, are you suggesting me to add bleache to the KI/I2 solution and then add to the bleach/KI/I2 the HCL? Or rather you are suggesting to flow Cl2 through my solution?

second:

if the solution contains I2 + KI one could simply add KCL to precipitate the already present I2??

thanks

Please use proper capitalization. Also, the proper nomenclature is HCl and KCl, not HCL and KCL, respectively.

"Add bleach to the KI/I2 solution and then add to the bleach/KI/I2 the HCl." That is correct. You are generating chlorine in-situ. It's the same thing as bubbling chlorine into the KI/I2 mix.

You won't precipitate I2 by adding KCl to your solution; it's a byproduct in the reaction that forms I2.

You are better off using H2O2 & HCL. add a little water to the iodine solution, about 25 percent of the solutions volume. thenn add a few milliliters of HCL. then slowly add 3 percent H2O2 while stirring until the solution starts to look milky. Let it sit for abou 45 minutes and the iodine will have precipitated.

It's pretty easy to screw up with bleach.

Enkidu, so the elimination of the I3--- from I-salt is the key for precipitation, right?
It is not the action of the byproduct but the removal of iodine salt to get the I2 off the solution... Am I correct? There was not capitalization to be written wrong, this time... :-)

Genocyde, I was not able to understand your issue.. 25% of what?solutions? What solutions?

thanks

Yes, as the potassium iodide is converted to iodine, the solubility of the iodine in solution will decrease. Be sure to boil off all the ethanol first.

I don't understand how it's 'pretty easy' to screw up with bleach... ?

Sorry... I shouldn't post while stoned.


Boil off the ethanol? You realize that I2 sublimates at room temperature don't you? There is no need to boil off the ethanol anyway.

Take the tincture of iodine, add water. The amount of water you add should be about 25 percent of the volume of iodine tincture that you are using. 100ml tintcure add 25ml of water. Then add a few ml of HCL (muriatic). Now slowly add 3 percent H2O2 while stirring until the solution looks milky. Let this mixture sit for 45 minutes and your I2 will precipitate. A big beautiful pile of long skinny I2 crystals will be laying on the bottom of the container.

Decant all the liquid down the drain. Add a little fresh water and pour the I2 into a filter. Now rinse the I2 well with fresh water while still in the filter. The best way to dry the I2 is to twist the filter, squeezing out most of the water. Now put the filter right in the middle of a whole newspaper and squeeze the hell out of it. Keep moving the filter around in the newspaper and squeezing until the filter no longer leaves a wet spot on the newspaper. Put the I2 in something airtight, and place it in the freezer.

Piece of cake.

I will try to dream about both methods. And I'm trying to guess the chemestry behind H2O2 method... but no idea!

Roy, I think he means:

H2O2 + 2 HCl - - - > Cl2 + 2H2O

Then the Cl2 reacts with KI as stated before;

2KI + Cl2 - - - > I2 + 2KCl

Pretty interesting idea there, as the chlorine stays (or should stay) as an aqueous solution eliminating the need to work with toxic chlorine gas.
I hope this helped. :)

Sublimation of the I2 will remove any chlorides formed by the bleach method... even then, if you get the 'ratios' right, you won't have many chlorides at all.

I dreamt i tried the H2O2 method. Maybe too much HCl or too much H2O2... Obtained a poor yeld and I think lots were lost during filtration process.
A bit of theory would improve this process. I don't like to dream to put something into something else without having at least a clue on what I am doing. I'm still looking around to find something.
Nevertheless, if someone knows something, he could advice us...:confused:

Why not just do what I suggested? Masonjar did the experimental work in that thread on DRO. If you need a 'recipe' then search the net... there are lots of recipes for both the H2O2 and the NaOCl methods.

Ive wade allot of I2 via the oxygenation method
Detailed Here on Frogfot's site
http://www.frogfot.com/synthesis/iodine.html

10KI + 2KMnO4 + 8H2SO4 ==> 5I2 + 8H2O + 2MnSO4

I can retain 90%+ yields using this method, I have tried many other methods but I find them tedious and I tend to like avoiding the exposure to CL2 gas when H2O2 is added to HCL (but that's just me)

I would strongly recommend sublimation at least twice! A few reactions I have ran with I2 seem to react with let over chlorine acid so I like my product clean

Here (NZ) our iodine tinctures use a PVP (liquid polymer?) solvent which, after one try with possibly decomposed H2O2 i had no yeild even though it was left overnight.
Is this because of the different solvent or just crappy H2O2?
Also the reaction with H2O2 doesn't involve chlorine AFAIK, its a textbook redox reaction: 2H(+) + H2O2 + 2I(-) --> I2 + 2H2O
So basically acid catylises an electron swap between peroxide and iodide, taking it out of solution as iodine.

You probably used bad H2O2; and besides you should have used KI or NaI, not alcoholic tincture of iodine. However, there is some tendency for liberated I2 to re-enter solution as the I3- anion.
BTW There is a current thread on this subject going on http://www.sciencemadness.org/talk .

Just thought you mite find it Interesting
I get my KI from horse specialists It is a supplement they give race horses.
Its expensive $55 for 500grms but per mol its still cheaper then I2

And if NZ is anything like Australia...
I would say that the Iodine tincture you are talking about (beterdine) is provodone Iodine which is 10% v/v but provedone only has like 10% v/v I2

And afaik you cant extract I2 from provedone or its very inefficient

Thats just how it is here...

In my country I can only find iodine tincture. It is 7g of KI and 5g of I2 in water/alcohol solution (couldn't find the ratios). By boiling of the alcohol (at 78°C) until the T° restared rise I obtained 2 things:

a harsh soring in my nose and eyes, and 20ml of solution with I2 precipitating out by itself.
I will perform the Cl2 method of course. I have to admit that the H2O2 method has the strong advantage of not needing a toxic gas flow.
Was PVP Iodopovidone?

Just thought you mite find it Interesting
I get my KI from horse specialists It is a supplement they give race horses.
Its expensive $55 for 500grms but per mol its still cheaper then I2
And if NZ is anything like Australia...(cut).
That KI given to horses is probably either analytical grade or pharmaceutical grade (USNF or BPC), which would also be veterinary grade. As such, it would be far more costly, involving recrystallization, than reagent or "technical"/industrial grades which may have bromide or chloride or other impurities. I wonder if farm supply stores have cheaper grades of the stuff, used as a supplement for animals other than racehorses in iodine-deficient areas.

I think that most NaI and KI probably comes from the sea, along with the bromides, as a byproduct of common salt extraction, being much more soluble than NaCl, but they would be very impure to begin with. The iodine and bromine are probably obtained from the brine left over by oxidation. There are also deposits of NaIO3, mixed with halides and nitrates, as caliche in the desert areas of northern Chile.

Iodine can be extracted from formulations (aka, stuff that contains unwanted crap) using copper (II) sulfate or similar copper (II) salts. In order to do this, the iodine needs to be in the I- state.

From wikipedia:

# In the laboratory, copper(I) Iodide is prepared by simply mixing an aqueous solutions of sodium or potassium iodide and a soluble copper(II) salt such copper sulfate.

# Cu2+ + 2I− → CuI2
# The CuI2 immediately decomposes to iodine and insoluble copper(I) iodide, releasing I2.[2]

# 2 CuI2 → 2 CuI + I2

This means that you need to add potassium sulfite or similar agents (many ways of reducing I2) to an aquous solution of 'contaminated' iodine until colorless, and then some. The insoluble CuI comes out as a dirty grayish salt but this is OK, even ACS reagent CuI seems to have this color. This salt is collected and the solution (once depleted of iodine) is discarded.

CuI cannot be dissolved in water but it can be oxidized in water regardless of this fact. I once added H2O2 and H2SO4 to CuI and iodine appeared, but there are really tons of ways to make I2 from I-.

I have seen bromine generated in situ in order to brominate stilbene. To 10mL of ethanol with 0.5g of stilbene dissolved in it, 1.2mL of HBr was added to the and then 0.8mL of 30% H2O2 was added. The method described above should work in a similar manner to generate Cl2 in situ to precipitate iodine.

Here is a link to a video showing the H2O2, KI, HCl process:
http://www.youtube.com/watch?v=CLhwkFKLdPA

Seems pretty straightforward and simple. (BTW thank Charles for the link, he referenced it in another thread).

This process is a plug for the new book by Make Magazine titled "The Illustrated Guide to Home Chemistry Experiments" by Robert Thompson. This book is perhaps the book I would have written had I written a book. Thompson is a man whose views closely parallel my own concerning the demise of chemistry in today's society. Check out his speech on the demise of the chemistry set here: http://blog.makezine.com/archive/2008/07/robert_bruce_thompson_on.html

Back to the iodine, there is a direct link to download the video from the publisher here:
http://cachefly.oreilly.com/make/WeekendProject10Chemistry.mp4

There is a page devoted to the video, and to plug the book, at the Make website in the weekend projects section:
http://blog.makezine.com/archive/2008/06/weekend_project_home_chem.html

Not only is potassium iodide an uncontrolled and unrestricted substance, but the fedgov actually gives samples away if you live with, I think, 50 miles of a nuclear power plant. You can also buy KI pills from a number of companies that sell it as pills for emergencies, although you will pay a premium price.

What the video did not show is how to purify the iodine to get actual crystals. This depends on what kind of reaction you need the iodine for, of course, but usually you don't want hydrochloric acid, hydrogen peroxide, and potassium ions contaminating your reaction. Filtering through a coffee filter will only be marginally effective as you would lose a considerable quantity of iodine. However, it works, and that is what really matters.

Megalomania, thanks for your opinion of the book "The Illustrated Guide to Home Chemistry Experiments" by Robert Thompson. I have been thinking about buying this book (I have only read online reviews from others) but was unsure if it was worth the price and contained good/proper information. I will buy it now.

I uploaded the MAKE- Blog (iodine video) Weekend Project- Home Chemistry.flv to the ftp.

It is in folder: UPLOAD/Phrankinsteyn.

I almost bought the book last week myself, but I thought about it later that evening while taking a walk and ran a prime projection... After I shell out my $30 of money I could better use elsewhere, I would just toss it on my stack of papers and not get around to reading it for a few months. I also know as soon as I buy it an ebook version will appear on Gigapedia, although I would prefer to have this in printed form. I will wait to buy this book until I have the time and inclination to actually read it. There is now 1 copy available via interlibrary loan, checked out and reserved for months in advance, so that might be an option once the dust settles and people stop reserving it.

The book is actually much larger than I thought. I saw the author flipping through the pages of the copy he was clutching in the iodine video. That thing is as big as a phonebook!

If anyone has a line on where a ebook copy can be obtained, let us know ;)

No ebook source, but the printed version can be had for $17.30 + $3.99 S&H from Amazon.

Thanks to the positive review, I just ordered it. Can't wait.

Just purchased a copy off eBay, looks like a great book :)

Received the book today, has a few experiments I must try. :)

Here are a few links from the book that may be of interest to some of the members here.

http://www.homechemlab.com/

http://forums.homechemlab.com/

newsletter address: hcl-subscribe@homechemlab.com

The book states that the newsletter is published sporadically and if possible subscribe using a "real" (ISP) email address rather than an email address from Yahoo, Gmail, or a similar free email service. If newsletter email to your address bounces, that address is removed automatically from the mailing list.

I read the thread you linked.

questions:

i read twice your post, enkidu, are you suggesting me to add bleache to the KI/I2 solution and then add to the bleach/KI/I2 the HCL? Or rather you are suggesting to flow Cl2 through my solution?

second:

if the solution contains I2 + KI one could simply add KCL to precipitate the already present I2??

thanks

I think you should confirm this with Meg or COP. Something doesn't sound right here to me. And those guys are pretty sharp. My knowledge is on a need to know basis. But it just doesn't sound right

This along with his video should do it (help people like me). :)

Here is the link and procedure (copied from) to Robert Bruce Thompson method of iodine production:

http://forums.homechemlab.com/viewtopic.php?f=8&t=3&sid=50e56bb635fd5d6f9ceb83825ac18e93#p3


Isolating elemental iodine from potassium iodide


Iodine crystals are used in a couple of the experiments in the book. When I wrote those sections, iodine was freely available, but the DEA recently moved iodine to List I, which means it now requires completing paperwork and showing ID to purchase iodine. Fortunately, there's a very easy way around this problem. You can isolate elemental iodine from potassium iodide, which is included in one of the chemical kits. To do so, take the following steps:

1. Weigh out 2.0 g of potassium iodide and transfer it to a test tube.

2. Add about 1.5 mL of distilled water to the test tube and swirl to dissolve the potassium iodide.

3. Add 1.5 mL of concentrated hydrochloric acid (or about 1.8 mL of hardware store muriatic acid) to the test tube and swirl to mix the solutions.

4. Add about 10 mL of drugstore 3% hydrogen peroxide. The solution immediately turns dark brown as the iodide ions are oxidized to elemental iodine, which precipitates out.

5. Swirl the test tube to suspend the iodine and pour the liquid through a funnel with a folded piece of filter paper to capture the iodine crystals.

6. Rinse the iodine crystals on the filter paper several times with a few mL of distilled water. The rinse solution appears brown from dissolved iodine, but iodine is not very soluble in water, so you're not losing much of your yield.

7. Spread out the filter paper on a watch glass or saucer and allow the crystals to dry thoroughly. Iodine gradually sublimates (passes directly from solid to gaseous form) at room temperature, so don't leave the crystals exposed to air any longer than necessary to dry them.

8. Once the crystals are dry, transfer them to a sealed storage bottle or vial.

These quantities produce a gram or so of iodine, which is sufficient for the experiments that require it. If you need more iodine, simply increase all quantities proportionately.

Robert Bruce Thompson
thompson (at) homechemlab (dot) com

Ah ha, I have been to that home chem lab forum. I thought it was just some spammers trap with all those numerous empty sections. This is the latest spammer trick, making fake blog comments and bulletin board posts on sites they created that makes it look like people are talking about the product. Porn sites are the most prolific in this regard.

Poor iodine. Now I have to jump through fedgov hoops and convince them I need iodine to kickstart Grignard reactions, not to dominate the world as a meth cook. Time to start buying sea weed...

Time to start buying sea weed...

Hahahaha... next you'll be trying to isolate a certain amine from gallons of your saved piss.

If we ever get a user-submitted content thingy working, I2 should be one of the tutorials.

I also just received "The Illustrated Guide to Home Chemistry Experiments" by Robert Thompson. It's laid out something like a course text in that it has a quiz at the end of each lab along with "Required Equipment and Supplies", "Substitutions and Modifications" and "Optional Activities" that delve a bit more into the lab at hand.

Interestingly, the individual labs are in many cases designed to give a useful result, like molar solutions, etc., that can be kept for supplying your home lab and not just tossed out at the end of the lab. It's a good idea to read ahead to the next lab before disposing of the previous lab's results because sometimes the results are used in the next lab (reminds me of my old Gilbert chemistry set in this regard).

Most if not all of the Guide's info can be found online but this has the advantage of being progressively ordered and all in one place.

But make no mistake- this is aimed squarely at the beginner, and you will find no labs for pyrotechnic devices or HE's, et al.

It advertised that the completion of this guide would be the equivalent of a first-year college general chemistry lab course, and is probably an accurate assessment.

Hey, for US residents the link below might contain useful for those intending to buy iodine legally, including pretexts for the purchase and warnings about suspicious behavior.

"The Comprehensive Methamphetamine Control Act of 1996 identifies iodine as a List II chemical. DEA mandates that detailed records be kept for sales of iodine crystals that exceed the threshold of 0.4 kilogram established in 2000. Anyone who sells a total of 0.4 kilogram (13.98 ounces) of iodine crystals to an individual, corporation, business, or other legal entity in a 2-month period must obtain data identifying the purchaser, keep records of the transactions for 2 years, and report any suspicious transactions to DEA. This rule does not apply to iodine tinctures or other iodine mixtures."

http://www.usdoj.gov/ndic/pubs1/1467/index.htm

Small irony here is, I just learned (from the above link) more about meth production than I knew previously!

If I were contemplating making this shit, I would be investigating "cold-cook" methods as well as having learned all I need to know in regards to research to prepare myself for scrutiny from a supplier of iodine.

Truth be known, I actually wish that meth could be eradicated. Too bad that the powers that be decided to make everything but the kitchen sink regulated towards that end- w/o actually removing the scourge.

Just saw 100g go for >$20/oz on eBay, even potassium iodide has gone through the roof. And just when I really need iodine to do some legit chemistry labs with:mad:...

This police site with suggestions on what clues to look for in spotting meth labs...or amateur chemistry labs for that matter. It can be reverse-engineered to provide security hints for the amateur chemistry on how not to arouse too much suspicion. Cops should be proud of their work, they're teaching us a lot.

http://www.qccrimestoppers.com/projectX.shtml

"Methamphetamine Labs

Quad City MEG Teams up with Crime Stoppers
August 16, 2004
Quad City Metropolitan Enforcement Group announced a new partnership with Crime Stoppers of the Quad Cities to locate, eliminate, and arrest those responsible for methamphetamine labs.

Methamphetamine is one of the most dangerous drugs officers encounter. This is due to the hazardous materials that are used to manufacture meth, along with the volatile environment a lab creates. Officers who respond to labs place themselves in an unstable environment that has the potential to injure them.

In response to the recent increase in labs, Quad City MEG and Crime Stoppers have started this awareness campaign. Billboars were put up in six locations around the QCA. hen a person chooses to start up a meth lab, he/she places the public, neighbors, children, the environment, and law enforcement officers in danger. Meth cookers need to know that law enforcement has a zero tolerance and that IF THEY COOK IT - WE WILL COME!!!!

If you have any information concerning a possible Methamphetamine lab, call the Crime Stoppers tip line, 309-762-9500. If your information leads to a felony arrest, you'll receive a cash reward of up to $1,000.

What are indicators of a clandestine methamphetamine laboratory?

* Little or no traffic during the day, but lots of traffic at extremely late hours.
* A strong smell that might resemble urine, or unusual chemical smell like ether, ammonia, or acetone.
* Extra effort made to cover windows or reinforce doors.
* Residents never putting their trash out or burning all trash.
* Lab materials surrounding property (lantern fuel cans, red chemically stained coffee filters, clear glass jugs, and duct tape).
* Vehicles loaded with trunks, chemical containers, or basic chemistry paraphernalia like glassware and rubber tubing.
* Laboratory glassware being carried into residence.
* Inhabitants smoking outside due to the fumes.
* Dying grass or plants in a particular area.

Business owners should be aware of customers who purchase or steal an excessive amount or a combination of the following items. Any unusual pattern of purchases of these items should be reported to police.

Acetone Aluminum foil
Anhydrous ammonia Brake cleaner
Camping fuel Coffee filters
Denatured alcohol Drain cleaner
Engine starter fluid Ether
Ephedrine/pseudoephedrine Products Funnels
Gasoline additives Iodine
Iodine crystals Iodine prill
Iodine tincture Lithium batteries
Lye Matches
Methanol Muriatic acid
Paint thinner Propane tanks
Red phosphorus Rubber tubing
Rubbing alcohol Sodium hydroxide
Sodium metal Sulfuric acid
Table or rock salt Toluene"

If the information in the last two posts is accurate, then that is a potential way to generate some income.

There is a legal 2 month, 0.4kg (about 14oz) limit to selling iodine (per buyer) - without needing any substantiating buyer information. Iodine sells on ebay for $20oz. Some additional number crunching is needed, but it sounds profitable. You would need to factor in the prices of potassium iodide, and H2O2, and the HCl. Set up a few shell e-bay accounts, and you're ready to go!

I just did a quick ebay search for crystal iodine, it seems the average price is about $30 for 100g. One guy has for sale 200g at $150! It says he ships daily (with the tracking info in 2 hours :rolleyes:), I wonder how much business he gets at that price. I have to wonder if any of the sellers are fevgov in disguise looking for meth cooks.

I just did a quick ebay search for crystal iodine, it seems the average price is about $30 for 100g.
A quick look shows the $28 price is for 28g! A cool C-note/100g.

The only "deal:p" is BIN for $53/100g, others are auctions that haven't ended. These auctions have been going for as much as $70/100g, as I indicated earlier.

I have to wonder if any of the sellers are fevgov in disguise looking for meth cooks.
Now, do you really have to wonder?;)LOL

One guy has a "newbie" icon w/a feedback score of 2 and NO other items for sale. Now if that doesn't send up a red flag...

Contributing to the resources on controlled substances, I'm submitting this list of prescribed quantities of precursors (status 2007):

http://www.dms.dpc.vic.gov.au/Domino/Web_Notes/LDMS/PubLawToday.nsf/b12e276826f7c27fca256de50022686b/db5b889aaa4657c3ca2573230000d01f/$FILE/07-84sr001.pdf

PS: Maybe this thread isn't the most appropriate place for the legal stuff I've been posting about controlled substances, but several searches didn't turn up a current ad-hoc thread.