Iodine
Obtaining
iodine
Crystal iodine - Sublimated flat flakes of dry
iodine I2, ready to weigh out and use.
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 , eye protection, gas
mask,
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
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
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.