Two semi failed attempts, maybe someone can help shed light on what to do next.

[Nick Delsignore]

Hello! I am new to refining and have done two semi successful runs. This is how the second one went:

1. I began by heating roughly 15 grams of 24kt gold filled shot until red. I noticed some of them turned different colors as if they oxidized.
2. After I flamed them, I put them directly in 70% nitric acid and distilled water.The solution let off reddish orange fumes, was exothermic, bubbled and turned transparent blue. I believe this indicates the presence of copper. (I had this soak for days before I moved to the next step)
3. Next I filtered it (using a vacuum filter), took the material with the filter paper and incinerated it with flux. (I did not let it dry before I incinerated. There were gold flakes stuck to black flux in my crucible so I chipped out as much as I could)
4. Then I put the flux and metallic material in a beaker with 25mL muriatic acid, added two mL of ZEP sulfuric acid (I read this can help drop lead) then added 15mL nitric acid. The solution turned green and most all the material dissolved.
5. I filtered it again
6. Added sodium metabisulfite to the filtered green solution, and it turned transparent brown, let off the same looking orange/reddish gas as at the beginning and a white precipitate appeared.

Here are my thoughts:

• The torch I used is a large butane kitchen torch, which might not be a good heat source.
• The nitric turned blue because of the presence of copper, and the aqua regia turned green because there was still copper present. The white precipitate might have been copper(I) oxide, and the brown liquid was still contained the gold. Or the brown liquid still had some copper dissolved in it, and the white precipitate contained copper(I) oxide as well as gold.

What happened? Where did I go wrong? What are your thoughts? What could I have done different? I am so lost...

 

[Brett Novak]

Don't feel bad, I've made this mistake also.

Nitric on it's own will not dissolve gold. But it will dissolve all the base metals. Except platinum from my understanding.

It may not be the "right" way to do it, but what I have started doing is starting with an AP solution of HCL and Hydrogen peroxide to dissolve base metals. (granted I'm working with PCB's and gold plated IC's, but I'd think it would work the same way.)

HOT method involves a lot of coffee pots and a hot plate, and takes about 24 hours to seperate the gold (in my case) flakes from everything else that goes into solution. Negative stannouse test, lots of recoverable gold flake in the bottom. If you have copper over gold, or something like that, I would think that it would work the same way and leave gold beads in the bottom.

LONG VERSION involves a 5 galloon bucket with 2 gallons of HCL and 1 liter of peroxide. Shake it every day, but again takes a few weeks in 100+ degree weather. Same results.

Then I do a few rinses, and an AR to dissolve the gold, chill, SMB and let it settle. Sometimes I get a "seperation layer" in the decanter and I re-run the thicker bottom stuff.

then again I'm only about 2 months into my experiments so what do I know.

 

[Akragon]

Hello! I am new to refining and have done two semi successful runs. This is how the second one went:

1. I began by heating roughly 15 grams of 24kt gold filled shot until red. I noticed some of them turned different colors as if they oxidized.
2. After I flamed them, I put them directly in 70% nitric acid and distilled water.The solution let off reddish orange fumes, was exothermic, bubbled and turned transparent blue. I believe this indicates the presence of copper. (I had this soak for days before I moved to the next step)
3. Next I filtered it (using a vacuum filter), took the material with the filter paper and incinerated it with flux. (I did not let it dry before I incinerated. There were gold flakes stuck to black flux in my crucible so I chipped out as much as I could)
4. Then I put the flux and metallic material in a beaker with 25mL muriatic acid, added two mL of ZEP sulfuric acid (I read this can help drop lead) then added 15mL nitric acid. The solution turned green and most all the material dissolved.
5. I filtered it again
6. Added sodium metabisulfite to the filtered green solution, and it turned transparent brown, let off the same looking orange/reddish gas as at the beginning and a white precipitate appeared.

Here are my thoughts:

• The torch I used is a large butane kitchen torch, which might not be a good heat source.
• The nitric turned blue because of the presence of copper, and the aqua regia turned green because there was still copper present. The white precipitate might have been copper(I) oxide, and the brown liquid was still contained the gold. Or the brown liquid still had some copper dissolved in it, and the white precipitate contained copper(I) oxide as well as gold.

What happened? Where did I go wrong? What are your thoughts? What could I have done different? I am so lost...

You're working with far to small of a quantity of gold to be recovered... learned this the hard way as well. Gold filled and plated, even rolled gold material is damn near impossible to recover anything from unless you have a huge amount... grams won't do it.

The gold will be in such small amounts that it will literally be transparent and will be lost... you may find flakes, but again this amount won't even be recoverable... it will disapear in your crucible or just go up in smoke

 

[Brett Novak]

Akragon is 100% correct on that as well. I'm running KILO's of raw material and getting grams out.... I didn't think about that.

 

[Nick Delsignore]

You're working with far to small of a quantity of gold to be recovered... learned this the hard way as well. Gold filled and plated, even rolled gold material is damn near impossible to recover anything from unless you have a huge amount... grams won't do it.

The gold will be in such small amounts that it will literally be transparent and will be lost... you may find flakes, but again this amount won't even be recoverable... it will disapear in your crucible or just go up in smoke

Wonderful, thank you so much. A few follow up questions:

I have been under the impression that anything labeled "gold filled" would be around 5% gold. Maybe that's not the case?
What happened during the reaction? Was I on the right track with my observations? Or maybe it was just because there was too little amount of gold, and I need to focus on building a larger collection of karat gold rather than gold filled.

 

[Akragon]

Wonderful, thank you so much. A few follow up questions:

I have been under the impression that anything labeled "gold filled" would be around 5% gold. Maybe that's not the case?
What happened during the reaction? Was I on the right track with my observations? Or maybe it was just because there was too little amount of gold, and I need to focus on building a larger collection of karat gold rather than gold filled.

Im not even sure IF gold filled would reach a %... Theres almost nothing there... And my guess for your experiment... like i said, just not enough gold present to be recovered

 

[Nick Delsignore]

Im not even sure IF gold filled would reach a %... Theres almost nothing there... And my guess for your experiment... like i said, just not enough gold present to be recovered

Fair enough. So what would be worth focusing on, karat gold or just incredible amounts of gold filled stuff?

 

[Shark]

I have ran as little as 3.5 gram of 1/12 10 karat gold filled and been able to recover the gold within .01 of the expected amount. It can be done, but you may need better equipment, especially filters. Even then, extreme care is needed to reduce losses. Even micro changes at each step can have drastic effects on the recovery.

These small amounts are similar to running an assay on ore or other materials.

 

[Brett Novak]

depends on your source.

I have an almost infinite amount of gold plated and gold based IC's and PCB's. Can't comment on gold filled, not into jewelry. Even then most of it will be gold plated with a base metal.

Buying scrap? Not worth it. You'll never make your money back. EVER....

Dumpster diving? Learn aluminum, brass, copper and bronze, then save all of your circuit boards and go through my list of steps. You can go one further and mechanically strip components and sort them, and sell to board sort. Older stuff has a lot of silver as well, which is a whole different beast. And then you have to deal with lead for anything pre 2006.

FWIW 100g of gold plated IC's in ceramic packages (so easy to deal with) yields about 1g of pure gold. unless you get nitric acid for free, anything less than Kg is not worth your time.

Sorry to sound discouraging - that's not my point. I've been scrapping for 30+ years and just got into gold recovery. For gold, my backyard looks like a meth lab LOL. But I scrap anything I can find, but it takes time.

 

[Akragon]

Fair enough. So what would be worth focusing on, karat gold or just incredible amounts of gold filled stuff?

it really depends on your goal... for me this is just a hobby. I've always loved chemistry... but never ever thought i'd find a practical use for it... amazing how life tosses you a bone once in a while!

Personally, i've played with plated and rolled/filled gold... its a waste of time unless you have tons of it. Silver is a little easier to find, and a lot cheaper to buy. You can refine a bunch of .925 silver with just a little Nitric, regular table salt, some lye, and table sugar... and bring it to almost .999 purity. I actually do that a lot more then i refine gold just because its easy and fun!

Gold on the other hand... its easy to get scammed... and expensive to purchase unless you get lucky. I won't bother with anything but karat jewelry, and i won't buy it unless it has a hallmark stamp. Though i have managed to get my collection of 24k gold up to 11g since i started doing this... and im getting pretty good at it too.

so again, it depends on your goals... but i wouldn't plan on getting rich... lol

 

[Shark]

Buying scrap? Not worth it. You'll never make your money back. EVER….

I must be doing something wrong then… I have been running gold filled scrap for over five years now. The worst I have done on a lot by lot basis is to break even. This was done as an assay type understanding for me. Since then I have had bad deals (where I only doubled my money) to great deals (where I have better than quadrupled my money). I invest from $500 to $1200 per lot average and do this two to four times a month. As for ewaste, it is where I started. I still collect it, but save it up for those rainy days and slow times. I still do some components, boards are mostly a waste these days, takes up too much room for the amount they return. Ship it to a refinery for better returns. One day I may take all this serious and go at full time, but for now it is a hobby that pays for my other hobbies.

Anyway, best of luck. Hope you get what you want out it.

 

[Akragon]

Figured i'd post a little Flex

 

[Brett Novak]

Oh I'm not saying it's not do-able. And yeah for me it's a hobby also.

But...

This was FREE minus work and chem's.

So flex away hahaha

 

[Brett Novak]

and I have another 15 gallons of solution to refine

I will post pics of my method in a bit when I have my transfer cable. Primarily for PCB and IC's.

 

[Shark]

Hello! I am new to refining and have done two semi successful runs. This is how the second one went:

1. I began by heating roughly 15 grams of 24kt gold filled shot until red. I noticed some of them turned different colors as if they oxidized.

Heat them until they stop smoking. To much heat may melt any lead used in making jewelry.

1. After I flamed them, I put them directly in 70% nitric acid and distilled water.The solution let off reddish orange fumes, was exothermic, bubbled and turned transparent blue. I believe this indicates the presence of copper. (I had this soak for days before I moved to the next step)

Leave it until the base metals are gone, or adding heat to 125F causes no more red fumes.

1. Next I filtered it (using a vacuum filter), took the material with the filter paper and incinerated it with flux. (I did not let it dry before I incinerated. There were gold flakes stuck to black flux in my crucible so I chipped out as much as I could)

This is not the time to melt it. It is still very dirty, with a lot of copper most times. Take the filter and contents to a clean beaker, cover with hydrochloric acid, heat to 125F or close to it, add nitric a few ml at a time. This reduces waste of your nitric acid, which is often expensive. Once all metals go into solution, add a few mg of sulfamic acid at a time until it stops foaming and bubbling, stir while adding. This replaces sulfuric acid at this point and does two steps at the same time. It helps to eliminate any excess nitric acid plus it reduces any potential lead in the solution. Excess nitric can keep your gold from dropping out. Allow to cool if necessary and filter until crystal clear.

1. Then I put the flux and metallic material in a beaker with 25mL muriatic acid, added two mL of ZEP sulfuric acid (I read this can help drop lead) then added 15mL nitric acid. The solution turned green and most all the material dissolved.

See previous reply above.

1. I filtered it again
2. Added sodium metabisulfite to the filtered green solution, and it turned transparent brown, let off the same looking orange/reddish gas as at the beginning and a white precipitate appeared.

Add a gram of sodium metabisulfite to 15 ml of hot water for every gram of expected gold. Pour this solution into your clear gold solution and wait for it turn brown. Allow to settle. Once settled to clear, siphon off excess solution leaving the brown gold in the beaker. Rinse with water until it is no longer acidic. PH papers can help with this, or rinse multiple times to be sure. Melting at this point can be done, if you looking for higher purity use another round of AR and repeat the process.

Here are my thoughts:

• The torch I used is a large butane kitchen torch, which might not be a good heat source.
• The nitric turned blue because of the presence of copper, and the aqua regia turned green because there was still copper present. The white precipitate might have been copper(I) oxide, and the brown liquid was still contained the gold. Or the brown liquid still had some copper dissolved in it, and the white precipitate contained copper(I) oxide as well as gold.

What happened? Where did I go wrong? What are your thoughts? What could I have done different? I am so lost...

Getting high grade gold can be tough, but not impossible. Maybe some others can chime in about the “washing” method to raise purity. If not I will try to find an old post that explains it. Or search “shiny gold” might be a bit hard to find, but tons of good info can be found in the search.

 

[Nick Delsignore]

Figured i'd post a little Flex
View attachment 58474

I'm loving all of the advice and photos!

So I think I may have bitten off more than I can chew by starting with gold right out of the gate.

Silver may have a lower barrier to entry. So for silver, what kind of scrap or product do you purchase for refinement?

This is also just a hobby for me. I love chemistry and do not expect to get rich. That's what my day job is for, hah!

 

[Brett Novak]

don't get me wrong - it isn't necessarily a difficult task but it's easy to be fooled what materials are actually what, what YOU figure out you can work with easily, and how much you want to spend.

For me, boards and IC's are plentiful, and I've worked out my process to good repeatability.

Also, once you have your gold seperated, how are you going to melt it? MAPP works but you can blow fine particles all over. I've got an electric furnace which makes it easy to do oz at a time instead of the torch. (I generally wait until I have a good amount ready to melt)

it's more than just chemicals, you need the torches and stuff too! But if you start with easier metals like copper and aluminum to get the melting side down, you are starting out better than jumping right to expensive stuff.

 

[Akragon]

I'm loving all of the advice and photos!

So I think I may have bitten off more than I can chew by starting with gold right out of the gate.

Silver may have a lower barrier to entry. So for silver, what kind of scrap or product do you purchase for refinement?

This is also just a hobby for me. I love chemistry and do not expect to get rich. That's what my day job is for, hah!

grab any kind of silver you can find, not plated... again don't waste your time. You can find Sterling (.925) at any thrift store or pawn shop... they will over charge you unless you happen to find something nifty at a thrift store, but keep in mind its just for practice. Even on Ebay you can find silverware easily at a very over priced state.

Just keep in mind although the process is quite a bit easier you'll still be using nitric, and lye which can be very hazardous if not handled correctly... also Sreetips is a great guy to follow on Youtube.... Hes basically the rockstar of refining these days LOL

 

[Brett Novak]

oh it's a blast and it gets addicting!

 

[Nick Delsignore]

grab any kind of silver you can find, not plated... again don't waste your time. You can find Sterling (.925) at any thrift store or pawn shop... they will over charge you unless you happen to find something nifty at a thrift store, but keep in mind its just for practice. Even on Ebay you can find silverware easily at a very over priced state.

Just keep in mind although the process is quite a bit easier you'll still be using nitric, and lye which can be very hazardous if not handled correctly... also Sreetips is a great guy to follow on Youtube.... Hes basically the rockstar of refining these days LOL

Thank you for validating that for me, hah!

Based on market rate for .999 silver, I priced sterling at around $.65 USD/gram.

Assuming that price, I am seeing tons of stuff all over ebay, but it all seems so incredibly overpriced or right at market rate. And people are buying it up like it's a deal. I get some of it has intangible value however I am looking for scrap to refine.

Where do you find deals on scrap silver? Or do you just take the hit, try to minimize the loss as much as possible and do it for fun?