# Iodine but with a twist. You wont believe it!



## DNIndustry (Nov 23, 2008)

Hey I know there are tried and true method of stripping and refining
Against some advise I kept looking employing Iodine as renewable stripper.
I stumbled across a patent that renewed my interest.
I mentioned in one of my posts that I used potassium Iodide and Iodine to strip. problem was that I had to watch and pull out as it hit the nickel substrate. U could tell despite my efforts the white cloud was nickel.

*This patent starts out talking about using hydriotic acid/iodine, but towards the end it mentions his real invention.
Using NH4I/Iodine.*
_Lou's edit: The addition of ammonium hydroxide (liquid ammonia) to iodine crystals will form an explosive compound called nitrogen triiodide. It is more sensitive than nitroglycerin and plenty powerful enough to remove fingers and send shrapnel at lethal velocities. DO NOT DO THIS UNDER ANY CIRCUMSTANCE. _

Lou is correct. I accidentally put nh4oh but the correct chem is NH4I. This is not dangerous. I do recommend a condenser apparatus to reduce values getting lost. The iodine metal complexs are able to be a vapor hence the (Van Arkel-Boer Process)
I constructed the bath precisely as instructed.
ran through 100 brightly gold plated socketed pins(amphenol 30 microns)
...
It doesnt even touch the base metal... I have to find my camera. They come out and the nickel substrate is so bright they look brand new. 
The pH is such that it only, pardon the pun, goes for the gold.
As well it works on Silver, Palladium, and supposedly platinum, rhodium, Etc. 
I dont have any NaBH4 ( $330 for 500g + hazmat shipping-Any sources?)

Its expensive to get the initial bath going.
451g Iodine crystals- about 17 Oz, but they are reusable.

Comparativly 1 gallon of cyanide stripper is saturated at 0.7 oz Troy
This solution is 4 ozt!

I am working on the precipitation as we speak, my pH meter died and it is absolutely necessary.

Here is the document....So far it works, Ill find a camera.


----------



## Lou (Nov 23, 2008)

Addendum: After reading the patent, the risk is not so high if all is done EXACTLY AS THEY SAY. I hope you followed the patent's recommendations to the T as failure to do so would cause serious problems. Frankly, that patent is utterly stupid. Iodine does work but it's also extremely expensive. Let alone the fact that buying large quantities of iodine (a DEA List 1 item) will probably get your house searched. Even though you have legitimate use, it will probably still be a pain in the butt and potentially lead to a house call from the most scary 3 letter agency for refiners, the EPA.

You should try this with bromine.

Lou


----------



## qst42know (Nov 23, 2008)

Anyone hear from DNIndustry yet? 

If things went wrong how would this be rendered safe? Or even can it be?

Can it be diluted or neutralized or would it have to be detonated where it sits?

Now I'm wondering if a list of mixtures or combinations to avoid would be prudent.


----------



## qst42know (Nov 23, 2008)

I'll have my fingers crossed. 

I did a wiki on the compound you referred to. In tiny amounts this is used as a chem class parlor trick set off by a touch of a feather?


----------



## Oz (Nov 23, 2008)

I used to make small batches, Lou is spot on as to sensitivity. If he did mix the 2 all one needs to do is wait, it will go off. A car driving by the house could do it, I have even heard of flash pictures setting it off.


----------



## Platdigger (Nov 23, 2008)

Not saying I have done it.......but what if you got sodium iodide together with ammonium hydroxide? Would this be benign?
Randy


----------



## Lou (Nov 23, 2008)

This prompted me to start and sticky "Situations to Avoid" thread over in Safety.

I'm just counting on his good sense to follow the patent to the word. That patent should never have been accepted written as it was (I read through the patent after my preliminary post); things could get out of order if there was but one deviation to the order of addition. 

NaI and ammonium hydroxide (really it's just ammonia) are benign to start with, but as the NaI eventually oxidizes to free I2, then problems arise with explosives. It should be a rule that ammonia water solutions should be kept away from free halogens. 


And yes, the material is that sensitive. It's fine if you make a few milligrams (well not from a legal perspective) for demonstration, but this material does not keep and it is incredibly dangerous to have in a glass vessel. I've seen it explode underwater for no apparent reason.


----------



## Pawnbroker Bob (Nov 23, 2008)

I personally witnessed this in my chem classes. Scary stuff. The prof always opened a new semister with respecting the chemicals and how dangerous they can be. He used a feather and at some point would put some wet material under the leg of a students chair before class. That was always a shocker when it dried!

PB


----------



## qst42know (Nov 23, 2008)

Last we heard from him he was on his way to get the camera.

As for me I can't wait to read your safety post Lou. And I do hope we hear from him soon. 

Anyone on the forum have his contact info? A phone number?

Have you sold him any supplies or videos Steve.


----------



## lazersteve (Nov 23, 2008)

No I haven't sold him anything.


----------



## qst42know (Nov 23, 2008)

For those like me that did not know what a free halogen was.

http://en.wikipedia.org/wiki/Halogen


----------



## DNIndustry (Nov 24, 2008)

sorry guys. Didnt mean to scare you. 

Im fine. 

A bit over dramatic but appreciated.


----------



## DNIndustry (Nov 24, 2008)

Im doing some research regarding this topic out of respect for safety and the respect you have shown me.

I followed the directions to a T.

I am hesitant to post this so edit accordingly Mods. My intent is to show that preparation is not the same. As the end product is not the same either. It does strip well. I plan on reducing the remains of what I have back to elemental iodine as laid out in the patent and making a smaller batch. Any pictures or references any one may have would be much appreciated. It is a great tool if it is safe. 

Powder some iodine fine, and
put a very little of it (about as
much as will lie on quarter of an
inch of the small blade of a knife)
into a small saucer. Pour in
enough strong ammonia water to
cover it, and let it stand for about
20 minutes. Then either stir the
powder up, and filter it (see CHEM-
ICAL EXPERIMENTS) or pour off most
of the ammonia, and then pour the
powder on a piece of blotting-paper.
Place the filter-paper or blotting-
paper where it will dry in the sun.
When it is perfectly dry, rub a stick
on the powder, or even brush a
feather over it, and it will explode
with a crackling noise. Though it
has not changed in looks, the iodine
has been made by the ammonia into
a very explosive substance called
Nitrogen Iodide. The reason why
so little iodine was used, is that
otherwise the explosion might be
dangerous.


----------



## Lou (Nov 24, 2008)

It is very good to know that you're OK. The way you wrote that I was seriously concerned. After I read the patent I was less worried. 

FYI, you can always just buy ammonium iodide rather than make it in situ. 

Made properly (and by that I mean to be the most unstable, true NI3 not the ammonia adduct that you could have possibly created NI3.NH3), it is so sensitive that you couldn't even move it if you even wanted to do so. Filtration is impossible, as is any manipulation.


----------



## qst42know (Nov 24, 2008)

Now that we know your safe where are the photos?


----------



## Shaul (Nov 24, 2008)

I remember some 40 years ago (as a teenager) making Nitrogen TriIodide as an experiment. It was so damn easy to make it was almost laughable. But once it dries, that's where it is. You probably couldn't move it more than a few feet without setting it off.

I remember one experiment where I had an empty cardboard matchbox with a piece about the size of a small bread crumb. I picked up the box at the end of a pair of long steel tongs and gave it a quick shake, there was a loud explosion and the box totally disintegrated. Sure taught me a healthy respect for explosives.

Ways to set it off: touch it with a feather/ shake it/ blow on it/ look at it cross-eyed/ think about it. 

Personally, I would bury this whole idea. I've seen enough people making mistakes with something simple like AP (by not following directions), without messing with one of the most unstable and volatile explosives around.

I can just see some guy writing in and saying: "Help! I mixed a kilo of Iodine crystals with a quart of Ammonia. It's sitting on the kitchen counter and it looks pretty dry. What should I do with it now?"

All this really needs is one bad accident and it could blow up in our faces(literally), and take down the forum.

There's enough good work coming out of the forum.

Let's put this one to rest.


Shaul


----------



## qst42know (Nov 24, 2008)

Hiding things like this would be irresponsible. Far more so than proceeding when you know its dangerous. Someone proceeding after being warned is a choice. Finding out by accident would be shameful. Shared knowledge is the root of safety. I'm not suggesting a recipe book be posted but knowing in advance what combinations to avoid would make for a far safer group.


----------



## jsargent (Nov 24, 2008)

That explains what happened to my neighbor's horse...

Seems the poor nag had got all scratched up in some barbed wire so Henry (my neighbor) doctored him up with iodine but I said "Henry that horse has tar all over his scratched butt from rolling around on that sticky spot out on the road... ya outta take some ammonia and clean him up." Well it was a dry day and that ammonia/iodine mixture dried out pretty quick-like....

Henry never quite got over it.


----------



## Shaul (Nov 25, 2008)

qst;

Over in the new thread ' Safety-Situations to Avoid ' you offered a number of excellent suggestions.

In light of that, I'd sure like to hear your take on working safely with Nitrogen Triiodide i.e. ; Preparation / Proper Handling / Neutralizing (of dried crystals) / and Proper Disposal (of same).

Remember, unlike Acids etc., this isn't something you can just drive down to the Hazmat center with.

Perhaps there are some of our members who deal with explosives &/or 'bomb disposal', who could offer real-life suggestions on dealing with this stuff.

And yes, a very possible scenario: You've prepared a quantity of it, you've observed all the safety precautions and it's sitting there in your lab or basement or garage (or even your kitchen) or wherever; among your acids and chemicals and glassware & stuff.

Suddenly you're called away on an emergency (could happen to anyone) and you can't deal with it for a day or a week, or longer. You come home to find it sitting there- dry as toast.

Now What???


Shaul


----------



## qst42know (Nov 25, 2008)

Shaul said:


> In light of that, I'd sure like to hear your take on working safely with Nitrogen Triiodide i.e. ; Preparation / Proper Handling / Neutralizing (of dried crystals) / and Proper Disposal (of same).
> 
> Shaul



Obviously there is no safe way to handle nitrogen triIodide. I know this because this knowledge was shared not because it was hidden. 

It would seem to be more dangerous to close the door on situations such as this. I feel it is safer to discuss conditions to avoid than it is to make them taboo.

Have you shared your take on safe refining?

It would seem ammonia is a major player in the formation of explosive compounds however it has legitimate uses in refining. As a wash of AR precipitates to remove silver (in my limited chemical training) I am unaware of a substitute. 

Is there one? 

Ammonia and silver oxide forms a similar explosive compound. Should this be hidden or discussed?


----------



## DNIndustry (Nov 25, 2008)

As of the original post I used 500-700mls. By used I mean I dissolved gold and added SMB to precipitate.
My pH meter took a crap on me so I have held off on processing until today- I got my new one. I want to be safe. No sign of my fn camera. Ill keep you posted. The nickel substrate looks brand new...But yes I know, proceed very cautiously.


----------



## qst42know (Nov 25, 2008)

Honestly Shaul.

I am not trying to push your buttons but this patent is incomplete. It presumes that those reading it are experienced chemists well aware of where the process can go astray. 

As it turns out DNIndustry knew of the pitfalls and avoided them. As someone who lacks the required experience, I and others need this input from those that do know to keep us safe. Incomplete processes are a danger to the rest of us.

DNIndustry.

Please continue. My apologies for cluttering your thread.


----------



## Shaul (Nov 25, 2008)

qst;

I'm not trying to push your buttons either.

I guess what it boils down to is putting out as much quality information as possible, posting warning signs (like you would around a fenced-in minefield); and then..'Caveat Emptor' : 'Let the Buyer Beware'.

Regardless, enough time and space has been wasted on this arguement.

I'm putting mine to rest.


Shaul


----------



## DNIndustry (Nov 26, 2008)

I have been wanting to post all friken day. 
I ran out and bought a cheap ass camera just to get some pics up.
Well cheep ass pics are what I got. 

I took what should have been some sweet ass pics. Not stabilization, ill work on getting a new cam but ill put up what i can.

This process showed me that i was about to throw away gold.
Since the ammonia/iodine doesnt touch nickel I can set it and forget it.
PH runs around 7.6 
I always thought the color of the contacts changed to this brown color once it hit the copper insides... Turns out its still gold. till i see shiny it stays in the bath. ive got close to 3,000g of heavy gold plate Thicknet contacts to process again.  

Doing the math 
1 gallon = 3.785411784 liters
1 gallon of bath will hold 4 ozt of Au|Ag|Pd|Pt|Rh
4 ozt x 31.103 g = 124.412g (before needing oxidizing)
3785.411478 mL / 124.412g = 30.42mLs/gram
or
47.335 mLs/ pwt
1 ozt = 946.70 mLs

This is based off the estimates in the patent. To be honest I am seeing slightly higher precipitation. Extremely fine metallic gold precipitation. not mud, but very obvious sedimentation that is a bitch to get out of plastic, clings to glass too.
I havent dried or weighed yet so I could be wrong...
I wish i had that fricken mass spec....Id love to run a sample.
Maybe that would be a sweet service I could offer if the douche bag ever comes through.
Testing for the board, any thoughts.?


----------



## DNIndustry (Nov 26, 2008)

well. So far no problems. I have been running sample sets of 35mls in 50ml centrafuge tubes. Works well. I got antzy and ran one of them all the way through...
I made my first button. Came out to just over a 1.5g which would support my math as prior posted. 

Lasersteve-Thanks for the videos, on the site! I got good info on the melting...I tried i 3x before with deep crucibles..bad luck. I only have a MAPP Pro/O2 torch here right now. I changed to propane. Actually worked better, followed the prep, but kept blowing the powder out. This time I tried a combo of your technique and Hoke, put it in as wet glazed the top put a little borax soap ( not actual sodium borate like before-works like shit) on top and put a lid on the crucible. I evenly cooked it until the i heard/smelled the soap melt ( good smell) removed the lid and circled the till i had a button. 

I did notice using the h2o2 at 35% during agitation actually causes some of the Iodine to precipitate. As part of my final washing I avoided the Nh4OH and went for H20+H202. This disolved any traces of Iodine precipitate.....
If any one is actually following this.
By the way the DEA regulations regardidng elemental iodine crystals is no more than 400g in one purchase. Hydroiodic Acid is controlled in all quantity.


----------



## EVO-AU (Dec 13, 2008)

To one and all: As a kid laborer in the mines way-way back, there was this gent from back east who used the above chemical makeup. Talk about powerful - wow - juice ( nitro ) didn't even come close. We sure did move a lot of rock.

Ah, history and no EPA and gov't agencies. EVO


----------

