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diddi
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is there any lit on preferentially crystallising the alpha form of ICl over the beta form? might be a nice little project
[Edited on 30-12-2014 by diddi]
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j_sum1
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@Ramium
I wouldn't boil it down first. The tincture has iodine in the form of the tri-iodide ion. You can think of it as a iodide ion I- combined with an I2
molecule. If you heat you could drive off the I2 as a vapour and your yield will be lower. On the other hand, if you oxidise you will have I2
precipitate since it is insoluble in water. This separates easily.
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Ramium
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Thanks for the advice.i did some internet surfing and found a differnt recipe using
HCL and H2O2 .this is the recipe
4 parts 2% iodine tincture to one part DH2O (distilled water)
You will also need .75 ml 30% HCL per fluid ounce of iodine tincture. You will need a container to hold all of the fluids you now have in front of
you. It doesn't matter if its a bowl, jar, beaker, or anything else. Just make sure to always use glassware.
You start out by pouring the iodine tincture into the container. Slowly add the DH2O and stir, but always avoid splashing. Then, slowly add the HCL
and stir.
At this point, you need to wait for about 15 minutes to let the reagents do their work. --- After you have waited 15 minutes, add the H2O2 slowly
while stirring. At this point, you need to wait for 12 hours. --- Now, you need to have a filter and another container ready. I recommend an ultra
fine plastic mesh cone filter. It won't clog, and it won't absorb any of the liquid. Sometime the color will be too dark, and you can add a bit more
H2O2 and let it sit for a second pull. Now you need to rinse the crystals that remain in the filter with copious amounts of water. After this, spoon
or tap them onto a stack of three coffee filters. Fold the filters so nothing can come out. Now take some paper towels and wrap them around the filter
and try to get as much of the moisture out as you can. The final step is to drop the still closed filter into a container with Damp-Rid or any kind of
moisture absorbing product. If you chose to add more H2O2, proceed in the same fashion for the second pull. Would this work? Sorry to keep asking.
[Edited on 31-12-2014 by Ramium]
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gardul
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maybe I am missing something here. But wouldn't it just be easier to use postassium Iodide as the source of idoine.
I just made you read this very pointless signature. How does it feel?
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morganbw
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Quote: Originally posted by gardul  | | maybe I am missing something here. But wouldn't it just be easier to use postassium Iodide as the source of idoine. |
People often like to take different routes to the same item, but, yes, I think so.
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CuReUS
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in nurd rage's video ,he adds sulphuric acid to KI solution to get Iodine
https://www.youtube.com/watch?v=2F_kPXbi2D8
but it never works whenever I do that(I never used an ice bath though,do you think that's important?) ,can someone tell why ?
so instead of adding sulphuric acid,I used to add conc nitric acid,and the colorless KI solution would instantly turn black,which made me believe
that I was getting iodine
but recently I learnt that nitric acid oxidizes iodine to iodic acid(HIO3) 
http://en.wikipedia.org/wiki/Iodic_acid
[Edited on 7-1-2015 by CuReUS]
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Sniffity
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It should be possible, but rather impractical to obtain the iodine.
However, to explore the science behind it..
Upon dissolving table salt, you should get a solution of Sodium Chloride and Potassium Iodide. If you were to bubble Chlorine gas through said
solution, the Chlorine would displace the iodide, forming Potassium Chloride. The Iodide would convert to Iodine, which should precipitate out.
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gardul
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I have always used the HCl and H2O2 method.
basically desolve KI in small amount of water and add equal amounts of HCl. Add three times as much Hydrogen Peroxide (3%) Stir. and let it sit for 10
to 15 minutes. Filter out the iodine let it dry.
While this may be a boring way I have found it rather affective since iodine is so restrictive here.
I just made you read this very pointless signature. How does it feel?
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morganbw
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| Quote: Originally posted by CuReUS | in nurd rage's video ,he adds sulphuric acid to KI solution to get Iodine
https://www.youtube.com/watch?v=2F_kPXbi2D8
but it never works whenever I do that(I never used an ice bath though,do you think that's important?) ,can someone tell why ?
so instead of adding sulphuric acid,I used to add conc nitric acid,and the colorless KI solution would instantly turn black,which made me believe
that I was getting iodine
but recently I learnt that nitric acid oxidizes iodine to iodic acid(HIO3)
http://en.wikipedia.org/wiki/Iodic_acid
[Edited on 7-1-2015 by CuReUS] |
Refer to Woelen's first reply in this thread. It is pretty nice.
Subject: Synthesis of Iodine from KI and sulfuric acid question.
[Edited on 8-1-2015 by morganbw]
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CuReUS
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morganbw
but I used 98% sulphuric acid on the KI solution . maybe my KI was not contaminated with KIO3 
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morganbw
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Woelens method
| Quote: |
Indeed, 30% acid does not oxidize iodide to iodine. Using conc. H2SO4 for oxidizing iodide to iodine also is a bad idea, because that reaction is
extremely messy and dirty. If you add conc. H2SO4 to solid KI, then you get a mix of HI, H2S, S8, I2 and SO2. This mix is extremely smelly and looks
dirty brown with yellow specks like bad shit. Isolating the iodine from this dirty 'shit' is not a pleasure at all.
A much better method is to dissolve the KI in 30% H2SO4 and then add dilute H2O2 to this. Try to add a slight excess of H2O2 and do this slowly while
stirring. At a certain point you will see lots of glittering particles of iodine forming in the dark liquid. If you wait long enough, then you see
that the liquid turns lighter and iodine settles at the bottom and another part of the iodine settles near the surface. You can pour the iodine on a
filter (preferrably use a sintered glass filter and if that is not available, then use a dense paper filter). The wet iodine then can be put in a
small beaker to which about three times its own volume of concentrated sulphuric acid is added. When this beaker is heated, then you can see the
iodine melting, forming a nearly black liquid, which remains under the sulphuric acid layer. After this step and solidifying of the iodine, you can
decant the acid liquid (which contains water and left over potassium ions and a small amount of iodine) and add another small portion of conc. H2SO4.
Heating again makes the iodine really clean. After cooling down you can decant the acid again and then rinse with a lot of water. Finally, you end up
with a piece of iodine, which you can wipe dry with a small paper tissue and then break down in parts with a glass rod. You can also keep it as one
piece. The iodine, produced in this way is pure enough for all practical home chemistry experiments and syntheses.
If you want the iodine really pure, then you can heat it and let it sublime on a piece of cold glass. I myself tried this, but I had limited succes, I
stopped the process, because I lost a lot of purple vapor.
The most tricky part of the process described above is the filtering step. You end up with a dark grey mud, which stains everything. Paper becomes
black, skin becomes yellow/brown (like you sometimes see with certain tobacco users) and clothes become brown. That's why the best results are
obtained with a sintered glass filter, from which you can easily scrape the mud. The filter itself is cleaned very easily by rinsing it with a dilute
solution of sodium sulfite or bisulfite.
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I was wanting you to see the process he used. It seems to be the best I have come across. Nothing about KClO3 in his first response, just the method
he uses.
[Edited on 8-1-2015 by morganbw]
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Yugen
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I once thought this was a good idea too, until I really looked into it. Check out this old textbook that explains how iodine was made back in "the
good ole' days"
http://babel.hathitrust.org/cgi/pt?id=uc2.ark:/13960/t3tt4gz...
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CuReUS
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| Quote: Originally posted by morganbw |
I was wanting you to see the process he used. It seems to be the best I have come across. Nothing about KClO3 in his first response, just the method
he uses.
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I saw that too. he says that it becomes a mess.But when I added the sulphuric acid,NOTHING happens.
no fumes,no black goo,no iodine ppt nothing 
but when I put nitric acid,the solution immediately turns black,but there are no fumes
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Ramium
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Its working!!!! I can see iodine crystals forming lots of them to
Yes! Yes! Yes! Yes! Yes! Yay!!!!!!!!!!!!!!!!!
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jhonthebaptist
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I made some I2 before with ammonium iodide tincture from the store. After I dried it, it was was about the size of a pea. I accidentally dropped it on
the floor and it exploded, more like a purple fire cracker. Nitrogen tri-iodide was somehow formed in the reaction mixture, So beware of that.
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blogfast25
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| Quote: Originally posted by jhonthebaptist | I made some I2 before with ammonium iodide tincture from the store. After I dried it, it was was about the size of a pea. I accidentally dropped it on
the floor and it exploded, more like a purple fire cracker. Nitrogen tri-iodide was somehow formed in the reaction mixture, So beware of that.
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Describe exactly what you did?
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jhonthebaptist
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It was years ago so Im a little foggy . I think I just acidified with excess sulfuric acid to precipitate the I2. When it hit the floor it was more
like a loud pop as opposed to exploding, it was a surprise for certain. Hope this bit of random info helps someone, for safety sake.
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blogfast25
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| Quote: Originally posted by jhonthebaptist | | It was years ago so Im a little foggy . I think I just acidified with excess sulfuric acid to precipitate the I2. When it hit the floor it was more
like a loud pop as opposed to exploding, it was a surprise for certain. Hope this bit of random info helps someone, for safety sake.
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That doesn't make a lot of sense: NI3 is prepared simply by combining NH3 with I2. An acidified solution of ammonium iodide tincture CANNOT contain
any free NH3.
[Edited on 30-1-2015 by blogfast25]
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jhonthebaptist
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well Im telling you what happened, not to sound smart. I know it dont make sense, but it happened. I know what you are saying is true and I have no
explanation HOW it happened but none the less it must have had some free ammonia in there before all the acid was added, thats all I cant come up
with. Please understand that Im not making this up and if you don't believe it then theres nothing I can do. I dont use iodine tincture any more for
iodine after that, the other tincture made with alcohol is fine and never had a problem when I used it. So I don't know what else to say.
here is the tincture that I used.
[Edited on 30-1-2015 by jhonthebaptist]
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blogfast25
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It's not a question of 'believing/not believing' you, only one of trying to get to the bottom of things.
| Quote: | | it must have had some free ammonia in there before all the acid was added |
In that case the original product would have contained some NI3. Also unlikely.
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gdflp
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I've used this brand before to isolate iodine, but using acidified peroxide instead of sulfuric acid. It doesn't actually have any free iodine in it,
it is a solution of ammonium and sodium iodides dissolved in ethanol. Some ammonia is dissolved in the ethanol to denature it, I don't think that NI3
can form from NH3 and iodides.
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blogfast25
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If it doesn't contain any free iodine how can it have antiseptic properties?
Using acidified peroxide to oxidise the NH4I to free iodine would not liberate any ammonia and thus also no possibility of NI3, which the Baptist
invokes for the exploding iodine.
[Edited on 30-1-2015 by blogfast25]
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gdflp
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Exactly, I had no issues with the synthesis. I have no idea why, but there is no significant free iodine in the solution, the ingredients on the
bottle are listed as "45% alcohol denatured with ammonia, ammonium and potassium iodides, and purified water". Search for "decolorized iodine", it
seems to be more of a folk remedy rather than actually having much of an effect.
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jhonthebaptist
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I may have used hydrogen peroxide and HCL. It was 5-6 yrs ago. I know what what happened when I dropped it, so it dont matter to me. dont really care
if you believe or not. You just need a reason to point your finger. I will tell you this, next time I see a potential hazard, or I have had
experience in a subject, I will remain quiet . Dont even know if it would have caused a problem with what I wanted it for. So for me this is the end
of this topic, go try it and run it through a mass spec. then you can see for yourself. just cause you dont know me, dont disregard the message. kind
regards and blessings
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blogfast25
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AGAIN, no one here is claiming they don't believe you, nor am I pointing fingers.
You made a very specific claim:
| Quote: | | Nitrogen tri-iodide was somehow formed in the reaction mixture, |
It's normal, desirable even, that on a science forum some will want to question that, or understand better what caused the explosion, especially since
as the circumstances in which you prepared the iodine do not seem conducive to NI3 formation.
If you can't understand that and decide, rather childishly, to take it personal then you have definitely chosen the wrong hobby.
[Edited on 31-1-2015 by blogfast25]
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