Aqua Regia process with nitric acid

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goldsilverpro said:
Harold,

Sounds like about a 5 gallon silver cell.

It wasn't that large, although I don't recall exactly how large it was. Were it not for notes I provided to the buyer of the refining business, I'd not even have the information at hand that determined the acid consumption. My guess would be that the cell held about 2½ gallons, total. I was never very interested in silver----it was a necessary evil, so I ran it.

Your figures come out to about 113 tr.ozs. per gallon of nitric, which is in the same ballpark.

Fact is, the amount I'd start with would consume almost the entire amount of silver, but not quite. I'd heat until there was no more action, then add a tiny amount of acid until I was satisfied with the traces of silver remaining, and the pH was acceptable. All of it went in the cell, including the undissolved bits of silver, which was just crystal from a previous refining. I think the 100 ounces/gallon is actually quite accurate.

Were you using reagent grade nitric? I was using technical grade, which is weaker. That could have made a little difference.

When I first started refining, I purchased some reagent grade nitric, but ended up using it almost expressly for making critical solutions. The nitric I was purchasing appeared to be of high quality, so I, like you, used tech grade with excellent results. I watched for the formation of silver chloride when making electrolyte, but that was never an issue. I, of course, used distilled water.

Were you using any water to dilute the nitric?

Absolutely! While I'm not a chemist, one of the things I've read about is the hydronium ion. When you introduce nitric to silver, you find that it does very little work. Even when heated, it doesn't attack the silver with gusto. Add the slightest amount of water and all of that changes. My total volume of silver nitrate/water was held to about a half gallon while being produced, but, of course, was diluted for the cell. If I allowed my solution to cool, it immediately grew silver nitrate crystals.

I may be completely wrong but, I can't really see how the fume condensation would make much difference. I don't think the reaction in the equation is reversible. But, something gave you a better yield than I was getting, so maybe the condensation helped.

It's been so long now that I don't have a clear memory of the things I'd experience, but one thing I seem to recall is that what little fuming I got was slow to leave the beaker. Fact is, I used the presence, or lack thereof, of brown fumes in the beaker to help identify when there was no further action. Like you, I have no clue if what I did was helpful, or not, but it did help keep the solution from getting contaminated from outside sources. I even kept my silver cell covered to exclude any dust that might settle.

Also, you probably lost more fumes than you realized, since they eventually leaked out through the spout area of the beaker.

I fully agree. Considering I was the only person to use my equipment, I was all too aware of the losses one experiences in refining. It's the reason my fume hood had a filter, which, for the most part, collected the majority of values that were lost from the vessels. While the amount of gold recovered from the hood wasn't large, as compared to the volume of gold that was processed, I recovered no less than eight ounces about every other year, and that was strictly from cleaning out the hood, that did not include the filters that were changed on a regular basis. You'd have to see how the hood was built to have this make sense. I had built a chamber for such material to accumulate, secure in the knowledge that there were losses. I should also comment that my hood was built entirely of asbestos, and was used for incinerating polishing wastes and filters from jeweler's benches. I have no doubt that some of the losses were from dusting in incineration, not just vapors.

I think some of the big guys collect the fumes and separately convert them back to nitric acid.

Yeah, that's what I was alluding to. Somewhere in my library, all of which is in boxes aside from the odd book, I have something that discusses that very thing. Given enough time, I'll finish the house I'm building and unload the boxes.

I did a search a while ago to see if I could find books and other information pertaining to refining, but came up only with the loose-leaf you and I discussed some time ago, the one about the seminar in California. Couldn't even find my two copies of Hoke's book! We have a huge amount in storage----and I'm not up to spending enough time to sort through all of it at this point.

Harold
 
You know it's funny, but i was just reading about a machine that covers some of what GSP and Harold are both saying. I think Harold will like the recovery system on this one. Take a look.

Some good process info to.


Thanks,
Ralph.
 
Hey Ralph,

I first saw that machine on the net 4 or 5 years ago. There's much less info available on it today, so I assume that it wasn't a success.

The process it uses is simple and most people on this forum could set it up cheaply, without the use of a high dollar machine. It simply involves inquarting with copper or silver, shotting, and parting with nitric. Some of you are using this process already. The parting is done with several fresh applications of nitric and the purity of the gold is said to increase with each parting. It is said that after 3 partings, the purity may reach 99.99%. However, in the pdf, this third parting wasn't tested.

The first two partings are said to be similar to those used in fire assaying. The first is weak to prevent the gold from breaking up. The second is stronger. In fire assaying, the first nitric is about 1 part nitric and 7 parts distilled water. The second is 2 parts nitric and 1 part distilled water. In the pdf, the first acid is boiled for 2 hours and, since the total cycle time is 6 hours, I assume the second acid is boiled for 4 hours. The purity after two partings is said to produce 99.9% gold. The details on the third parting aren't given.

I have grave doubts that three partings will produce 99.99% gold. Maybe that's why this machine seems to have fallen by the wayside.

The Refining Machine Police
 
goldsilverpro said:
I have grave doubts that three partings will produce 99.99% gold. Maybe that's why this machine seems to have fallen by the wayside.

The Refining Machine Police

I've said that right along. Achieving 4 9's is not accomplished easily----although one must keep in mind that the industry standard is only 9995, which, in my opinion, is achieved with diligence.

Aside from the nice stainless reaction vessel(s), I see no particular advantage to buying a machine when the processes involved are identical to that which I have espoused. Think Hoke, and you have the entire process covered in fine detail.

Harold
 
GSP said:
The Refining Machine Police
8)

I love the fact that we have such an experienced membership here, it makes me feel all warm and fuzzy inside!!!

Thanks for looking out for all of us GSP.

Harold said:
Think Hoke, and you have the entire process covered in fine detail.

Well said Harold! Hoke has documented the pioneer work for all us in great detail.

Steve
 
The man enjoyed it so much. He said it twice.

:D :D :D

I wasn't impressed by the machine much. It was the way it captured the fumes and converted them into usable products. Plus with this it seems the losses from evaporation's would be nearly impossible. I know Harold
is a vocal supporter of this issue. I like things that go from a to b , and are both automated and environmentally friendly. The company still makes the product i think. I will email them for a pdf. I like to collect info anyway. :D

Thanks,

Ralph.
 
Ralph,

I found this same document about a year ago. I put a copy into my refining documents folder back then.

Steve
 
That's a picture of the stained glass window we had made for the castle. We removed it and brought it with us when we moved to Washington, where it now resides in our stereo room, on the front of the house.

It's a compilation of my wife's maternal coat-of-arms, and the coat-of-arms of the country of Greece (I'm American born, but of Greek heritage). Where the two lions stand, there would be two cavemen had we not altered it. We created our own design to reflect our heritage.

The crown is the logo I used in my refining business. You can see it here in the picture of the ingots I posted some time ago.

Harold
 

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Harold,

The window is magnificent. I love the design of the crest, it's very medieval. I'm into making my own armour from the medieval period. Every few years at Halloween I'll suit up in my armour and hand out treats for the kids in full garb. They enjoy it and we get a kick out of there reactions to the suit.


Steve
 
lazersteve said:
Every few years at Halloween I'll suit up in my armour and hand out treats for the kids in full garb. They enjoy it and we get a kick out of there reactions to the suit.
Steve

You'd have fit right in with us, Steve.

The window in question used to live in the round opening you see above the front door of the castle. The plywood you see was removed and a back lighting provided (fluorescent). There was a sheet of white acrylic plastic between the light and window to diffuse and make the light uniform. It looked really pretty at night. We left the light on at all times.

Harold
 

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alexmaywood
I skimmed through a couple times looking to see if anyone mentioned always using stannous testing solution before throwing away solutions. If not look in the testing part of this forum!

Wayne
 
I'm trying to dissolve a impure 14 gram button in AR. I've flattened it and cut it up as small as I can get it. I started with 100mls of 1 part 70% nitric and 3 parts 38% HCL. When it stopped bubbling I assumed it was done. Most of my gold was still in the bottom. I precipitated and got maybe 1 or 2 grams of black gold powder. I put the remainder of the gold to 200mls of AR and it has stopped bubbling but still lots of gold undissolved. Am I not using enough AR? If I heat it will it start again? Do I have to break the gold up more? Any help on this would be greatly appreciated. Thanks, Dave.
 
Is it possible the gold is alloyed with a large portion (30-80%) of silver? If so it may not be dissolving due to silver chloride formation. Do you see a crust forming on the gold? If a crust has formed and it darkens on exposure to light it is most likely silver chloride. Inquarting will free the gold from the silver.

Steve
 
Do your gold turned black ? If it's the case, you probably have silver alloyed. If not, I would recommend to try to heat it.
 
No nitric can't dissolve gold. Melt silver with gold until your gold is about 30% of the total weight. Then put the nugget (if you flatter it, it will dissolve faster) in nitric acid. Very weak nitric acid won't work good. Use 35% Nitric acid or more. You can heat it if you want to speed up things. But be careful with fumes and hot nitric !
 
Most all karat gold contains silver. You have to heat the AR to even have a chance of dissolving the gold. If you don't have a fume hood, this will be very fumey.
 

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