| Author |
Topic: Home-made I2 |
Osmium Member |
posted 05-27-98 02:09 AM
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
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
Brilliant....now if the RP was only as easy to make...hmmm. ;-)
|
Osmium Member |
posted 05-28-98 02:52 AM
I'm working on it ;-)
|
Osmium Member |
posted 07-01-98 04:41 AM
Hope you'll find it now, jimwig.
|
jimwig Member |
posted 09-30-98 05:42 PM
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
Os,
Do you have a work-up method for this now?
-drone #342
|
300
Spartans Junior
Member |
posted 10-17-98 05:20 AM
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
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
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
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
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
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
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
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
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
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
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
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
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
|