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Iodine

Obtaining iodine
Crystal iodine - Sublimated flat flakes of dry iodine I2, ready to weigh out and use.

Bilbo writes
I am fortunate regarding the I2 I live in Cow Country its no biggee at all to buy it and lots of it.
If I could throw something in to the mix here, when purchasing the I2 from the feed/tackle store, ask the rep about it quite casually. "My quarter horse has a big black rotten hole in its hoof, the vet/farrier told me some iodine crystal packed in the thrush hole would burn it out. How exactly do I apply it?" or something to the like. Reps have mundane shitty jobs and a chance to impart some of their wisdom is always well received.
If you are walking in semi dumb up front chances are you won't be grilled about intended purpose at all.
The straight iodine poultice is considered out of date medicine, many now go with bleach solutions because there are certain contraindications that can be suffered by the animal due to iodine exposure.
If the sales rep mentions this it will be important that you say the vet said the thrush is so
advanced if not treated right away and drastically the animal could suffer lameness**
Failing all of this like Worlock said in another thread.. mail order $45/pound
The shortest distance between two points is a straight line! (just make sure a trusted friend is the second point of that line)
Luck
Bilbo

Polar pure iodine - looks like small bee bee's used to purify water, this works great.
 


Converting iodine tincture
Tincture of iodine is iodide salts in alcohol, it is found in supermarkets in small one ounce bottles. Each bottle can generate a little over a gram of  I2 the price has shot up from 0 .60 cents to $1.80 / bottle. Tincture comes in 2% or 7%.
It is also available at feed and tack stores in pints and gallons.
Mail order through horse breeders supply magazines.
Safety #2    When making Iodine from tincture Wear chemical resistant gloves ,  eye protection, gas mask,work outside,  Work over newspaperin case any falls you can easily save it

Formula one
 1 pint 7% tincture iodine
3 pints of hydrogen peroxide
 2 oz of HCl
1/2 cup of d-H20

Shake it up,  in a one gallon jug,
Wait  20 minutes
Filter  through a pantyhose
Wring out fluids.
Put iodine crystals in a glass jar,
Re-wash four times with distilled water,  cover, shake, pour off the water into a filter
On the final water wash, wash the iodine into a into a fresh filter,
Wring it out hard,
Open up filter roll into a dry filter
Wring out hard
Put crystals in a dark place to dry.
Use a Drying agent like Calcium Chloride store with the  I2 in a sealed chamber
Grocery stores, for mildew prevention near the moth balls
I2 is light sensitive and will degrade.
When completely dry store in light resistant container..

Formula 2
4 part Lab Procedure as follows.

materials
1) 1000 ml  2% Iodine tincture  =  2.5%I+2.5%KI in etOH and H2O =-
2) 250  ml  Muriatic acid =  34.4%HCl
3) 475  ml  Hydrogen peroxide = 3% solution of H2O2
4) 1750ml  Distilled H2O

In a 1 gallon   container (plastic or glass),
mix  1 liter of  2% tincture of iodine
with 250 ml of Muriatic acid
stir and allow to sit for 15 min.

Add 475ml  of a 3% hydrogen peroxide
stir and let sit an additional  15 min.
Add 1750 ml distilled H2O
shake and let sit for  15 min more.

An orange water layer appears on top of a dark gray layer of  I2.
Pour off most of the the orange water

Add fresh distilled H2O  shake and let sit
Pour off most of the the orange water
Wash a total of three times with distilled water

On the last wash pour the I2 into a stack of 5 coffee filters
Wring it dry
roll the iodine ball into 5 dry coffee filters
Wring it dry
 Roll it into 5 more dry filters
wring it dry

Put the I2 in a small clean glass  jar break up the iodine ball
place the jar of  I2 on a piece of cardboard, cover the I2 with a larger jar
put in freezer for several hours
Remove  jar of  I2,  seal it tight, with cellophane then screw on the cap  store it in a dark cool environment
 

Mothballs
Amazing that someone would catch moths and put their balls in a box to sell?

Potential problems Not rinsing the I2 enough with water to remove the chlorine and salts from the tincture Not drying the I2 out enough and adding it too wet to your reaction. If in doubt at all re-wash the iodine with distilled water in a filter and wring out, The iodine is only very slightly soluble in water, you lose very little washing with water. If it is not clean and dry you can lose a lot more in a failed reaction.
 

The Solution
There are only three chemicals involved in the reaction, make sure they are top notch and your OK
1.  Ephedrine - the free base reacts stronger  than the HCl salt
2.  Iodine  - use more if you are not getting  a reaction 1(E)  :  2(I2)
3.  Phosphorus-  use more if doing a small amount    1(E)  :  0.8(RP)

 It hurts to see a couple of hundred dollars in chemicals go to pieces in front of your eyes..
So do not get fiendish and attempt a flawed batch, think first, before acting rashly

Sublimating Iodine-


 
 
 

Cold Finger - used to sublimate iodine from a flask. Is the way to purify your Iodine crystals.
The theory is that as iodine is heated it skips from a solid to a gas
when cooled it returns from the gas directly back to a solid.
Several test tubes are used. When one becomes damp from moisture, it can quickly be replaced,
preventing  water vapor from messing up your crystals.
Acetone and dry ice are used for the real cold finger you may need

This device using the flask and test tube is one method. A bowl and a plate do not allow you to easily chill ,collect, deal with water condensation, protect against iodine  vapor escape, or add more iodine to be sublimated
 
 
 
 
 
 

Red Phosphorous
Red Phosphorous






The Role of Phosphorus in Industry
There are seemingly countless uses for phosphorus and phosphorus compounds in industry. By far the most important of them is in the manufacture of fertilizers, a practice which uses up over half of the phosphate rock consumed in the U.S. About 15% of the phosphorus equivalent in phosphate rock utilized in the U.S. is converted into elemental phosphorus, the majority of which is used to produce phosphoric acid. In addition, some of this elemental phosphorus is used for a variety of military applications as well as in roach and rodent poisons. Red phosphorus, of course, is used to produce wooden and paper safety matches, where it is applied to the abrasive surface upon which the safety match is scratched. It is also used in the manufacture of fireworks.
 

Phosphates, especially polyphosphates, "are truly chemicals of universal application." [11] They have been used in baking powder, carbonated beverages, dental materials, dentifrice, detergents, fertilizers, fire resistant textiles, laundering, metal surface treatment (rust proofing), milk and milk products and water treatment, to name a few. 11 Phosphoric acid is used to flavor soft drinks, to defecate and clarify sugar, to manufacture gelatin, and to prevent spoiling in silage. It is also employed in the electropolishing of stainless steel and aluminum, as well as in other metal treatment applications. Finally, among other things, phosphoric acid has applications in the textile industry, in glass manufacture, in the purification of hydrogen peroxide and in a host of laboratory applications.

Taken from the 1993 Aldrich catalog handbook
 
 
 CAS Compound Descrip Amount  Price 
7664-38-2,  Phosphoric Acid 85% soln. water ACS 500 g  $ 12.90 
1359-36-2,  Phosphorous Acid 99%  500 g  $ 19.40 
7723-14-0  White Phosphorus 99+% in water 100g  $ 71.50 
7723-14-0  Red Phosphorus lump 99.999% 25 g   139.00 
7723-14-0  Red Phosphorus powder 99% 500 g $ 23.80
1314-56-3  Phosphorus pentoxide 98+% ACS Reagent 500g  $ 25.80 
6303-21-5  Hypophosphorus Acid 50% wt. soln. in water 500g $ 26.40

 
 

It is not illegal, in all states but it is watched just like Iodine and large amounts of ephedrine.
Get some and you will always have some, not much gets used  up, it does become coated with organics
you can clean those off easy. You can re-use it over and over again.

No, you cannot get it out of picture tubes on TVs
Yes, you can get it off match strikers
Yes, you can get it from road flare strikers
Yes you can walk into a Chem. supply house and buy 4 oz for $50
Yes you can mail order it to your business for very much cheaper. $95 for 2 kilos
Yes it is found in fireworks
If you can get over this hurdle your headin' for the finish line.
Ask, beg, or buy the information on where to get it for it from anyone you can, you will get some.
It is out there, others do it so can you. Keep after it, eventually someone will tell you where to get it.
Amorphous Red Phosphorus 99.5% pure,
Help out a dealer, ask him to ask the cook where to get it. No one wants to tell, it is a secret.,
I once had someone walk into a Lab supplier and buy 4 oz. Now some people bring me kilos every now and then
Mail order from on the web, check the posts in the hive


Cleaning Red Phosphorous
This is a proven,  no BS procedure for cleaning up RP. This is not the procedure used to get the RP off of match strikers.
The use of Sulfuric acid and/or Hydrochloric acid  is recommended only in severe cases if nothing else will work.
What happens to the RP,?  Some gets oxidized in the reaction and is gone. Most will get a waxy build up after a few uses,
It gets course and grainy because the powdery stuff,  is what reacts the best,  large surface area for a small volume.

Screen
Run it through a fine stainless steel  screen, (kitchen utensil - grocery store) to remove debris, and breakup chunks
Acetone
 put the RP in a funnel with coffee  filter   pour acetone through it until the acetone is a light yellow

Solvents
Any of the following familiar solvents have been safely used to wash the RP
methanol, ethanol, denatured alcohol , isopropynol, toluene , xylene
Rinse with acetone again to remove non-polar solvents

Water
Final Washes  with warm or hot distilled water

Sulfuric acid wash  (rarely needed)
If the RP still has an abnormal  coating
Soak in warm dilute H2SO4 10 minutes
Add equal amount of HCl for 10 minutes
let settle
pour off the acid
repeat until clean
repeat the Acetone and water washes
Dry it
An oven at 150 F  to 200 F just barely on,
I have had the glass bowl break while baking  1/4 pound of RP in the oven , the RP was fortunately still wet , it started to smolder about 15 minutes later  the house was full of smoke.
Threw the towel on it , that slowed it down, pumped two large  fire extinguishers into it with no effect , secured the garden hose and with wet towel finally put it out, began the clean up and there was still areas on fire, the extinguishers ruined the RP and made a nasty mess
Screen and powder
Usually screening it will be is enough ,
Powder with mortar and pestle
 

References:
1. Latimer, W.M. The Oxidations States of the Elements and Their Potentials in Aqueous Solution. Prentice-Hall, Inc. New York, N.Y., 1952. 105-112.
2. Bard, A.J., et. al., eds. Standard Potentials in Aqueous Solution. Marcel Dekker. New York, N.Y., 1985. 139-161.
3. Frost, Arthur A. J. Am. Chem. Soc., 73, 2680-2682. 1951.
4. Wagman, E.D., et. al., eds. The NBS Tables of Chemical Thermodynamic Properties. v. 11. American Chemical Society. Washington, D.C., 1982. 2-38, 2-74 and 2-75.
5. Gould, E.S. Inorganic Reactions and Structure. Holt, Rinehart and Winston, Inc. New York, N.Y. 1962. 249-257.
6. Weast, R.C., ed. CRC Handbook of Chemistry and Physics. 70th ed. CRC Press, Inc. Boca Raton, F.L. B113.
7. Sillen, L.G. Stability Constants of Metal-Ion Complexes: Inorganic Ligands. Burlington House, London. 1964. 179-203.
8. Jolly, W.J. The Chemistry of the Non-Metals. Prentice-Hall, Inc. Englewood Cliffs, N.J. 1966. 89-106.
9. Hayward, P. and D. Yost. J. Am. Chem. Soc., 71, 915 (1949).
10. Nyquist, R.A., C.C. Putzig and M.A. Leugers. Infrared and Raman Atlas of Inorganic Compounds and Organic Salts. Academic Press. San Diego, C.A., 1997. 206 and 209.
11. Standen, Anthony, et. al, eds. The Kirk-Othmer Encyclopedia of Chemical Technology, 2nd ed. v. 15. John Wiley and Sons, Inc. New York, N.Y. 1968. 269-70 and 290-92.