distilling nitric

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I use gallon pickle jar in sand bath, with teflon lid turned on lath & hole for tubing, clear hard plastic tubing chemical resistant, not sure of type but we use it to pump chemical for water treatment to the boilers at work, I coil this tubing in bucket of ice water for condenser, this same bucket of ice water is what the reciever jar sits in, I use teflon tape then electrical tape then cloth tape to seal reaction vessel, also tie down the teflon lid with wire to prevent pressure from pussing off lid, wire tie's to handles of the aluminum pot for sand bath. a hot plate for heat source.
CAUTIONS :
do not change temperature on glass rapidly (thermal shock)
only fill boiling vessel one quarter full
do not use rubber nitric eats it

this works great for me.
 
I am going to build a flange to mount to the flask ( a real flask) coil copper cooling line silver brazed to ss condenser so water can run all the time - basically the same as lab ware but made by me on the cheap from ss.

Jim
 
james122964 said:
I am going to build a flange to mount to the flask ( a real flask) coil copper cooling line silver brazed to ss condenser so water can run all the time - basically the same as lab ware but made by me on the cheap from ss.
You can also put a larger diameter piece of tubing around the stainless condenser tube, held in place by two discs. It could be copper or stainless. An inlet and discharge on each end, on the sides, provide for water circulation. I built my retort that way---it worked very well for distilling mercury.

The exterior tube insures complete heat transfer, something that might be a consideration when using stainless, which is not a great conductor of heat. The assembly was silver soldered.

Here's a poor picture of the retort, which shows the cooling tube and connections for cooling.

Should you pursue a similar design, make the bottom the inlet with the top the outlet. That way you're assured of the chamber being full of water at all times. I used a small submersible pump and a 5 gallon bucket for my water supply.

Harold
 
Am I missing something? A copper cooling line and silver solder for distilling nitric.
 
It's all very acceptable, Oz. It would be used strictly for the cooling circuit. The nitric would be eposed only to stainless.

Harold
 
Does anyone know the lowest concetration of nitric acid that is usable to remove silver and copper from inquarted gold? Is 10 percent feasible given no hurry for reaction to complete?

Also, under my name says expert gold refiner, I am not, could someone remove or change it to hobby level?

Thanks
Jim
 
James,
I too have tried to have my description changed from "gold refiner" back to " member " several months ago to no avail. Now I am an " advanced gold refiner"! :D
I would prefer mine to just say member.

Mark
 
lol, the description under your name is based on how many posts you have, not your actual refining level. All the phpbb forums have it. Consider it a badge of honor, I do. If I give advice on anything, I am sure to point out that I'm new at this too. I just have a big mouth and like to type :) But if I didn't talk so much, I wouldn't have so many friends on here either. :!:
 
I don't like misrepresenting myself.
Don't get me wrong, I do know how and have done a bit of gold refining , but, keep in mind that most of the gold mined from N. Ga is already pure enough for the gov't.

I try to learn about the pgm's and ,... if I get any info that I think anyone would be interested in, I pass it along.

At this point, I'm just a hobbiest .

Mark
 
2NH4NO3 + H2SO4 --> 2HNO3 + NH4SO4
ammonium nitrate fertilizer and sulfuric acid,
little excess sulfuric would probably benifit reaction.
since (NH4)2 SO4 boils at 100 deg C,
and HNO3 boils @ 83 deg C,
and excess H2SO4 will form NH4HSO4 right away,
and if distilling Nitric Acid with Ammonium Nitrate,
I assume the HNO3 boils first before Ammonium and if temperature is controlled the NH4 would not contaminate Nitric acid,
or maybe a way to test and remove residual ammonium from the acid?
Ammonium Nitrate fertilizer would be the cheapest.
and I have used it but always concerned about ammoinia portion in my recovery methods,when using this for nitric.

LOU or anyone Here have any ideas on this?
 
markqf1 said:
James,
I too have tried to have my description changed from "gold refiner" back to " member " several months ago to no avail. Now I am an " advanced gold refiner"! :D
I would prefer mine to just say member.

Mark
I moderate another forum, one that includes machining, welding, casting, and live steam (model steam locomotives).

Early in the board's career they used to catagorize readers by the number of their posts, just as this board does. It can be very misleading----for some folks that may have considerable knowledge are chary of sharing what they know, while thers may have little knowledge but run their mouths (fingers, in this case) overtime, spewing garbage of little or no value. We have readers of both kinds on the other forum, and here as well.

From the above comment, you can conclude that the number of posts often has no relationship with the amount of knowledge contained in their heads, or of their willingness to share what they know, assuming they know anything.

Unless Noxx decides to turn off that feature, it behooves each reader to not make assumptions based on that arbitrary title. It often does not represent the person in the least.

Harold
 
Mark
I moderate another forum, one that includes machining, welding, casting, and live steam (model steam locomotives).

Harold, sounds interesting - what forum? If I may ask.

thanks

Jim
 
It's not a BIG deal.
Everyone that has been been here long enough, knows what the deal is.
I guess I'm guilty of talking so I can say something instead of talking because I have something to say. :D

Actually, I have had many questions answered here and that is why I return frequently.

But, I freely admit that I am no expert of anything to everyone.
My advice is free but should be considered for what it's worth.

Mark
 
If you wanted to know what I know about looking for gold in the mountains, I would tell you what I know from experience.

On the other hand, what I know about the tricks of the trade about gold refining, came from here.

Mark
 
I have managed to leach nitric acid from calcium nitrate and sulfuric acid.

I mixed concentrated battery acid - boiled off to half of the original volume
then after cooling added to calcium nitrate, instant reaction forming white precipate. Placed this blob of acid and calcium sulfate into a homemade glass funnel that has glass wool losely packed in the neck. Then slowly sprayed with water to leach out the nitric.

repeat with the using the leached acid to improve the concentration.

I ran the leach trough 3 runs.

Not to waste the nitric left in the calcium sulfate I rinsed and stirred it after leaching with excess water that will be my starting water for the next batch.

Not saying this is the best way, but it works without distillation.
 

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