Ammonium iodide-iodine solution

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j200

Member
Joined
Sep 3, 2012
Messages
7
Anyone tried the ammonium Iodide-iodine leeching solution? Taken from US patent 5137700. I'm having problems with it. I can't prepare it when I follow the patent.

An aqueous solution containing 400 gms of ammonium iodide was prepared as follows:

(1) 500 ml of de-ionized water was placed in a 2-liter beaker.
(2) 351 gms of iodine were added.
(3) 47 gms of hydrogen peroxide were added and stirred.
(4) 97 gms of ammonium hydroxide were slowly added and stirred until all the iodine dissolved.
(5) 100 gms of supplemental iodine were added and stirred until the deep dark brown solution formed and all the iodine had dissolved.
(6) The dark brown solution was then diluted to 1-liter.

I follow step 1 and 2. My hydrogen peroxide is 35% so I ad about 134 grams after which I add 97 grams of 25% ammonium water. All the iodine should dissolve but it doesn't. I need to add loads of hydrogen peroxide, like 300ml to make it dissolve but even after it's all gone, when I add more H202 there's still a vigorous reaction. If I add more ammonium water there is also a reaction occuring.

Anyone has any experience with this particular leeching solution?
 
Be careful with Iodine and Ammonia. The can form an ultra-sensitive and powerful explosive. I have a scar on my left hand from when a glass vial of Water with only a few milligrams of the compound exploded spontaneously as I was holding it.

This is not something to fool with, unless you understand the process intimately.
 
j200,There are much easier ways to process the types of material's your working on, the iodine leach is normally used for ore.

If I were you I would spend some time on the forum, and reading Hokes book, and learn the methods used to recover gold from these materials, spend some time understanding how to refine and recover before you begin to try it, Hokes book has some getting acquainted experiments, which are very helpful in understanding the processes you will be using later.

In the general chat section, read the welcome to new members, and the general reaction list, and the guide to the forum, from these you will gain many ideas, this will also help you get an idea of the many processes used and which ones are best for certain materials, it will also give you links to other information, and help you on the journey of learning the art of recovery and refining of these precious metals.

In the safety section read dealing with waste, and other post dealing with the safety issues you face.

I have only done very small experiments with the iodine leach, so I am unable to give you help you with this batch.
 
Use the following procedure for preparing Ammonium Iodide
Reagents : Due to vigrorous reaction, All should be deluting with water if they are conc. solution, that is
H2O2 use 3% - 6 %
NH4OH less than 10 %
Iodine : will add in very small increment
Procedure:
1) Put small quantity of I2 ( 2-5 grams) with some water in beaker
2) Using Dropper : add some drops of NH4OH
3) Using Dropper : add some drops of H2O2 , chemical reaction occur immediately. You will see Iodine start to dissolve , Oxygen Bubles and Heat.
(note :Depend on amout of reagents, if they are in excess purple fume will be.)
4) Looking at yours solutions :
-If it is red that mean you need to add more NH4OH and should be done before chemical reaction is stop ( Still seeing bubles). If it's stop repeat step 2
-If it is clear or yellow solution you can add more Iodine as in step 1 until it goes red and follows steps 2) and 3) and 4) again and again

Stop process when you get enough clear or yellow solution. Put it in new
beaker and then start new batch until no more iodine to process.
Finally, Place beaker contains NH4I solution in water and boiling to expelled excess ammonia. Untill there's no ammonia odor, your solution is ready for use to mix with supplement iodine to make NH4I3
Hope this should be help you
 

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