gold filled in aqua regia

hey guys ran into trouble, had a bunch of gold filled rings and chains and tried to refine it in aqua rigua ,everything was going well untill i added smb. when i went to see my mud it was pure white.

any ideas ,maybe add hcl to purify,

any help would be great

hollywood

For those of you who are following my lab experiments, I wanted to show this photo of a new step in the process that I am very pleased with.
This is scrap gold including: jewelry, low purity buttons, small placer flakes with mercury stains, and even some dental gold. What I did was melt it in the furnace and immediately pour the molten gold into a 5 gallon bucket of cold water. As soon as the gold hits the water it breaks into small jagged pieces that are mostly fairly thin. That is exactly what I wanted because all of this will be going into the Aqua Regia and the acid reacts much more quickly and thoroughly to small thin pieces of gold rather than say, a solid wedding band. I will weigh this before and after it goes into the acid, but most of it was 14K so I expect only about an ounce or so unless I add some -20 mesh flakes to the mix.

By droping the gold into water I exposed a lot more surface area and that's why my next step was to put everything into a nitric bath on the hotplate and let it simmer until all the fumes were gone. I drained off the liquid and dropped in some talbe salt to see if there was any silver. I got quite a bit of white precipatate which I believe to be silver. Hope this helps. ......russ

Opps....wrong photo. Here's the one that goes with that last post.

You would be far better served to learn to use the process of inquartation for processing high grade materials. While what you presented will work under ideal conditions, the presence of too much silver creates problems that are never ending, resulting in considerable frustration in being unable to dissolve your materials. You'll come to realize that the "corn flakes" that are generated by your process will have thick sections that will refuse to dissolve. You also have considerable trouble separating the gold chloride adequately from silver chloride, without generating a huge amount of fluid that must be evaporated. My recommendation is to avoid that process.

Please consider the fact that silver and gold can NOT be in solution at the same time in acid, with the exception being a miniscule amount of silver that behaves like gold. This concept has been well documented by Sir. T.K. Rose in his book, The Metallurgy of Gold.

Silver and gold can be in solution simultaneously in cyanide.

Harold

PRECIOUS METALS HERE

WOULD THIS WORK ON GOLD FILLED AND 10-14-18 KT GOLD

WOULD THIS WORK IR YOU DROP IT IN NITRIC 50% WATER 50 %
INQUARTING

PM

PM,
I think inquarting is alloying (melting together) with enough silver to make it possible to use nitric to seperate the gold from the silver. When a gold/silver alloy has too little silver in relation to the gold, nitric will not atack it. Making a seperation with nitric dificult if not imposible. Hence the need to inquart (change the alloy). I am sure Harold can elaborate....
Randy

PRECIOUS METALS said:

PRECIOUS METALS HERE

WOULD THIS WORK ON GOLD FILLED

Click to expand...

Please lose the "all caps" posting. It is considered shouting---which is bad manners when conversing with those that are your friends.

Processing gold filled objects is best done by simply dissolving the base metal in nitric and water until all of the base metal has been dissolved. Once it's gone, the remaining solids, once separated from the solution, can be dissolved in AR with success. The gold alloy layer tends to be quite thin, and is also somewhat cleaned of silver on the surface by the first dissolution with nitric, so the gold will easily dissolve in AR before an impervious layer of silver chloride can form, preventing the values from dissolving.

It isn't uncommon for gold filled objects to be bonded with lead based solder, so it's a good idea to allow the nitrate solution to cool prior to attempting to recover any silver that my be present. Lead nitrate will self precipitate from a cool solution, so the lead can be separated from the solution before any silver might be recovered. If there's any doubt about what has been precipitated, remember, it will dissolve in hot water, so if you choose to precipitate the silver traces with salt, wash the resulting chlorides in hot water to eliminate traces of lead.

AND 10-14-18 KT GOLD

Click to expand...

While alloys of gold can be processed directly with AR, it requires conditions that may not be convenient for the home refiner. One of the important qualifications is that the gold must be prepared thin enough to be completely dissolved before the silver chloride layer can form. Silver chloride can be expected from yellow or green gold, although rose and white gold may dissolve fairly well. The problem with this process is that you do not separate the base metals from the gold until you precipitate-----so the resulting gold will have considerable contamination from dragdown. If you don't care about gold quality, it is an acceptable process, although I don't endorse it.

WOULD THIS WORK IR YOU DROP IT IN NITRIC 50% WATER 50 %
INQUARTING

PM

Click to expand...

Your question is not clear. Please rephrase.

If you are not familiar with inquartation, make mention of the fact. It's an important part of extracting gold when it's alloyed with silver.

Harold

Hi harold, I also had a problem with the aqua regia method.
The gold filled necklace disolved nicely. i neutralized the acid, and then strained the acid. Then after it was strained I added sodium metabysulphate.
I have all white powder on the bottom.Once settled, I added boiling hot water and the solution turned yellow. I once again decanted the solution and kept rinsing the powder until it turned a reddish. I figured at this point that copper was present so I added some nitric acid. The solution turned blue. once settled most of the powder I had initally started with disapated in the water. Any ideas what went wrong ?

Iron, and base metals, sounds like your problem, using a technique not well suited for your low value scrap, also another problem you have is you do not understand what Hoke's book teaches, have you read it? If so, reread it.

you do not use sodium metabisufate to precipitate gold.

Hi Kaserta!

Maybe the problem is because you added sodium metabisulFATE, instaed of sodium metabisulFITE.

Take care!

Phil

Hi phil, I did use sodium metabisulfite. This is the process i used. I place a piece of 18k gold filled in aqua regia. That worked well. IT totaly disolved the entire contents. There was no sludge, grains or metal at all in the solution.
I then added urea to neutralize the aqua regia and strained the blue solution through a filter. I then added sodium metabisulfite to the solution and a thick white powder formed in the bottom of my glass jar. Then i added hot water and the solution turned gold color with particales of an oily substance floating on the surface which looked like copper. I continued to repeat the process 5 times with hot water. It seems the more often I added water the more the white substance diluted in water. I did this until nothing else disolved. Then I added nitric acid to the residue to eleminate any coppers, and or silver if any left. Then I washed the material once more, and allwed it to dry and melted the powder. The contents that were melted formed into a deep red substance which contaminated my flux. The problem here is that I do not know where my gold went. I have 3 more lbs of gold filled items to refine. I am seriously thinking about just putting them in nitric and allowing that to do its work on the base metals. I have some already in nitric and the solution is already turning blue which means the presence of copper correct?
Thanks
Gerry

kaserta said:

Hi phil, I did use sodium metabisulfite. This is the process i used. I place a piece of 18k gold filled in aqua regia. That worked well. IT totaly disolved the entire contents. There was no sludge, grains or metal at all in the solution.
I then added urea to neutralize the aqua regia and strained the blue solution through a filter. I then added sodium metabisulfite to the solution and a thick white powder formed in the bottom of my glass jar. Then i added hot water and the solution turned gold color with particales of an oily substance floating on the surface which looked like copper. I continued to repeat the process 5 times with hot water. It seems the more often I added water the more the white substance diluted in water. I did this until nothing else disolved. Then I added nitric acid to the residue to eleminate any coppers, and or silver if any left. Then I washed the material once more, and allwed it to dry and melted the powder. The contents that were melted formed into a deep red substance which contaminated my flux. The problem here is that I do not know where my gold went. I have 3 more lbs of gold filled items to refine. I am seriously thinking about just putting them in nitric and allowing that to do its work on the base metals. I have some already in nitric and the solution is already turning blue which means the presence of copper correct?
Thanks
Gerry

Click to expand...

blue solution? we learn through experience.remove base metal before you dissolve the gold.refining is a two step process.(1) reclaim the gold,separate gold from base metal.(2) refine the gold,dissolve the gold and precipitate leaving contamination's behind.using AR to dissolve raw material (gold bearing base metal) is a problem just waiting to happen.separate gold from base metal by adding material to 50% nitric acid and placing on a heat source.you should know when the base metal has been dissolved because the gold will be liberated and moving freely.

kaserta,
It is good you have the sodium metabisulfite. Not meatabisulf-ATE, these chemicals are similar but do not react the same way in solution.

Really I am trying to help you learn, and know how to deal with any problem you run into.
Here is my suggestion to help you, forget about getting a few grams of gold from what scrap you have now, spend time collecting more scrap while you learn, building your stockpile, right now I feel you will lose more gold than you will get if you keep going down this road being not totally sure of how to do this.

Study Hokes book, spend time doing all of the getting acquainted experiments she tells you to do, learn how to make stannous chloride and use it.

While you are doing this you may also go to Laser Steve’s Website and study all he provides, also study processes on the forum.

Pick a very simple process study it well (like acid peroxide and then HCl/bleach method using memory fingers), learn everything you can about it, then do the same for other processes or materials later.

Recover your gold and refine it to high purity without losses, and melt that beautiful gold and show it to us for us to admire.

This would be a lot of work but you would find it worth it, you would know how to deal with anything you run into.

These I copied from Palladium's signature line, you should find link to Hoke’s book and other good information in them:

The difference between stupidity and genius is that genius has its limits. Albert Einstein
1. Refining Precious Metal Wastes C.M. Hoke http://tinyurl.com/mfnyhs
(REV) (Free Download)
2. Get the (FREE) Gold Refining Forum Handbook VOL 1 here >> http://tinyurl.com/nyutnp
3. Get the (FREE) Gold Refining Forum Handbook VOL 2 (Final) here >> http://tinyurl.com/y9w5y73
4. Chemistry Handbooks Here (FREE) >> http://tinyurl.com/n27pqu
ALL FREE-----ALL THE TIME

Hope you the best.

Thank you for all your help.

butcher said:

kaserta,
It is good you have the sodium metabisulfite. Not meatabisulf-ATE, these chemicals are similar but do not react the same way in solution.

Really I am trying to help you learn, and know how to deal with any problem you run into.
Here is my suggestion to help you, forget about getting a few grams of gold from what scrap you have now, spend time collecting more scrap while you learn, building your stockpile, right now I feel you will lose more gold than you will get if you keep going down this road being not totally sure of how to do this.

Study Hokes book, spend time doing all of the getting acquainted experiments she tells you to do, learn how to make stannous chloride and use it.

While you are doing this you may also go to Laser Steve’s Website and study all he provides, also study processes on the forum.

Pick a very simple process study it well (like acid peroxide and then HCl/bleach method using memory fingers), learn everything you can about it, then do the same for other processes or materials later.

Recover your gold and refine it to high purity without losses, and melt that beautiful gold and show it to us for us to admire.

This would be a lot of work but you would find it worth it, you would know how to deal with anything you run into.

These I copied from Palladium's signature line, you should find link to Hoke’s book and other good information in them:

The difference between stupidity and genius is that genius has its limits. Albert Einstein
1. Refining Precious Metal Wastes C.M. Hoke http://tinyurl.com/mfnyhs
(REV) (Free Download)
2. Get the (FREE) Gold Refining Forum Handbook VOL 1 here >> http://tinyurl.com/nyutnp
3. Get the (FREE) Gold Refining Forum Handbook VOL 2 (Final) here >> http://tinyurl.com/y9w5y73
4. Chemistry Handbooks Here (FREE) >> http://tinyurl.com/n27pqu
ALL FREE-----ALL THE TIME

Hope you the best.

Click to expand...

butcher said:

These I copied from Palladium's signature line, you should find link to Hoke’s book and other good information in them:

The difference between stupidity and genius is that genius has its limits. Albert Einstein
1. Refining Precious Metal Wastes C.M. Hoke http://tinyurl.com/mfnyhs
(REV) (Free Download)
2. Get the (FREE) Gold Refining Forum Handbook VOL 1 here >> http://tinyurl.com/nyutnp
3. Get the (FREE) Gold Refining Forum Handbook VOL 2 (Final) here >> http://tinyurl.com/y9w5y73
4. Chemistry Handbooks Here (FREE) >> http://tinyurl.com/n27pqu
ALL FREE-----ALL THE TIME

Hope you the best.

Click to expand...

When I click on the tinyurl links for the Forum Handbook volumes, I get a nasty warning about it being likely to harm my computer. Anybody else get the same message? The Chemistry Handbooks link goes straight through to Scribid without any warnings.

Todd

I made a very good batch of nitric acid. The fomula I used was 4.5 cups water. 1.5 pounds 99.9% nitric crystals and bolied it all until it was disolved. Then i let it cool. then added 1 in a quater cups of 99.8% concentrated sulfuric acid slowly, and let settle overnight outside at 39 degree temps. then I brought it inside to let it get to room tempreture. No crystals appeared in solution at all.
Instant reaction to metals and disolves instantly. I use first for metal treatment before finish aqua regia process.

TBarrow said:

butcher said:

These I copied from Palladium's signature line, you should find link to Hoke’s book and other good information in them:

The difference between stupidity and genius is that genius has its limits. Albert Einstein
1. Refining Precious Metal Wastes C.M. Hoke http://tinyurl.com/mfnyhs
(REV) (Free Download)
2. Get the (FREE) Gold Refining Forum Handbook VOL 1 here >> http://tinyurl.com/nyutnp
3. Get the (FREE) Gold Refining Forum Handbook VOL 2 (Final) here >> http://tinyurl.com/y9w5y73
4. Chemistry Handbooks Here (FREE) >> http://tinyurl.com/n27pqu
ALL FREE-----ALL THE TIME

Hope you the best.

Click to expand...

When I click on the tinyurl links for the Forum Handbook volumes, I get a nasty warning about it being likely to harm my computer. Anybody else get the same message? The Chemistry Handbooks link goes straight through to Scribid without any warnings.

Todd

Click to expand...

Google has us on a black list. lol
It's safe.

quick question. I washed all my cpu pieces in nitric 3 times. then washed the parts with hot boiling water 3 times. I made aqua regia and have all the pieces soaking. It looks as if there is a minimal amount of silver salt that formed in the bottom. Before I continue to precipitate my gold, any suggestions on how to rid the remaining silver salt before I drop my gold precipate. Should I filter the salts out and rewash in nitric and restrain ?

Have you eliminated free nitric acid? You should do this if not.

Let these silver salts settle, decant (siphon or pour off solution into filter, do not disturb powders) filter solution (if gold this solution should be a nice yellow color), (copper in solution will make it green).

Save the silver salts after washing in boiling hot water, store them wet.

kaserta said:

I made a very good batch of nitric acid. The fomula I used was 4.5 cups water. 1.5 pounds 99.9% nitric crystals and bolied it all until it was disolved. Then i let it cool. then added 1 in a quater cups of 99.8% concentrated sulfuric acid slowly, and let settle overnight outside at 39 degree temps. then I brought it inside to let it get to room tempreture. No crystals appeared in solution at all.
Instant reaction to metals and disolves instantly. I use first for metal treatment before finish aqua regia process.

Click to expand...

The problem in in this step. If you didn't remove a large volume of sodium sulfate salts by precipitating at -5 degrees. These salts will show up to cause problems in any further processes.