Your advice (please) to validate my strategy

[ZiegenSauger]

Hello friends, hope this message finds y'all safe and healthy!

I have been learning, studying, reading, watching videos, practicing, experimenting, making lots of mistakes for some years now. Whatever the level I achieved today is because of the massive information available in the forum, help from many of you, and (informal) mentoring from Mr. Sreetips/Kadriver.
O consider myself good with Silver, and a prentice level with Gold (and others). I have been very successful with Silver, and, more recently, quite successful with Gold as well. Today I am able to recover Gold in very small quantities, from old mistakes I saved the solutions/papers, scrap, etc.
Considering the most common and easy processes in Hover's book, I am doing a decent job today

After this "brief" intro, I have an interesting situation I am not confident with:
- one lot of gold-filled jewelry (some scrap, some in perfect condition, some made with pure - most likely 18K - gold) - 50 g total received "as is"
- one lot of gold-filled watch bands (I verified with my computer-connected microscope, took images, and verified each one of all those pieces individually - 353 g of bands received "as is"
- after cleaning (removing all parts that, visually, had not gold), the net scrap weight was 152g including Karat Gold-filled and pure Karat gold pieces.
- I split into two batches: one all magnetic and the other absolutely no magnetic
- Incinerated
- Dilute HNO3 cook
- Filtered
- Washed clean
- Second bath in dilute HNO3, now both batches combined.
- Just for curiosity - it is not my main concern - Gold recovery (and now refining) is Hunky Dory.

What's making me scratch my head is:
- From the first diluted HNO3 cooks, I have produced two "sub-products" of the process, now in their respective beakers
- I filtered both thoroughly
- The first is the standard blue we all get in this phase. Stannous negative for everything, I put apart with Copper sheets, it is surprisingly dropping good Silver.
- The second, is a deep green solution, and here is the deal: POSITIVE Stannous for Gold.

Keeping in mind I am a stannous result below the average reader, the dark purple blew my mind off. There are several discussions talking about finding dissolved Gold in HNO3 solution, but still, should not happen.

Anyway, I decided to add Copper sheets to this beaker too. It is dropping this shade of black grain. Differently from the Silver drop, where the Silver grows out of the Copper sheets, this sand sort of quickly grows but almost immediately goes to the bottom. Also, the process is slower than the Silver dropping.

Do you guys agree I took the right steps here?

Now I can filter out the sand in a couple of days, wash it thoroughly, and go all over the steps again.

Any recommendation, advice, criticism, correction?

Based on my mistakes plus what I managed to recover from the leftovers, I assume I lost around 5g of Gold for being a stubborn learner with gold fever. I want to avoid losing anything if I can. I am a bit confused, a bit concern about the Stannous result and this dark precipitation.

Thank y'all in advance, sorry for the novel.

Cheers!

ZS/PH

 

[Topher_osAUrus]

I think thats a pretty solid idea.
But, one or two things that are sticking out to me is -18k gold needs inquarted so it doesnt cause problems... like, not allowing nitric to dissolve constituents. If one of those is silver, then you will make a silver chloride crust when you are attempting AR. But, you can gamble and may get lucky and have no silver in its alloy.

When you say "bands" did you just throw the whole thing in there? Or did you tediously separate the caps off of each link on the band?

Gold got in your solution from some free chlorine somewhere in the process. Probably the water you used to dilute the nitric. Chlorine is everywhere, really
Its probably very little gold in there. Leave the copper to cement it out. Then go from there.

 

[ZiegenSauger]

Thank you Topher_osAUrus , thank you very much indeed!

Yes, I took the tedious process to separate one by one of the caps, from all 350 g in bands . Thinking of the gold, it was even funny during conference calls and stuff

All the cleaned gold is in AR ("obviously", the two K bracelets are in pristine condition). AR has been running all day, just popped up the heat with 1-2 mL of HNO3 to see if any reaction. There is only some dirty at the bottom, most likely whatever residues were left from the last incineration.

One solution has finished - filtered the cement Silver out and put it back in Copper, nothing else happened.

The other solution is still "sparkling" (minuscule, but looking close with a magnifier it is possible to see something still reacting with the Copper).

Let me see how it goes, I will update you on the other side.

Most of all, really appreciate you taking the time to advise.

Cheers

 

[ZiegenSauger]

Hello Friends,

O collected between 3-5 of Gold from AR (since I am on the first refining, waiting to finish to have exact measure). It is within the predicted, hopefully, it is confirmed at least 3 g, so I will be on the profit side.

Here I added 4 photos of the other part of the batch, after the drop with Copper was finished. While washing, it was easier to see the color clusters: clearly, ~20% is Silver, the rest is about half a deep green, and half some shade of black). There is well over 5g of material, these pictures are from the microscope.

The last picture is the one that is intriguing: I most always drop Silver with Copper sheets when recovering from Sterling and other Silver alloys, Usually, when removing the Copper from the solution, there is a thin layer of Silver which I spray and it falls down quite easily,

For this monster, there was this deep green cover, not even with a stronger spray it would clean, but you can see, in the holes for example, that the dark cement was grown out of the Copper. Now, after dried, it partially cleans up leaving the same shade of black particles.

==> I am assuming this deep green is not oxidizing Copper since I never found evidence of oxidized copper with this tone of green.

 

[1mysurveymail]

You have two solutions of AR correct? One Blue, one green. Is your stannous test showing gold in both solutions? You never mentioned "De-noxxing" your solutions with a small amount of sulfamic acid (grout cleaning crystals). What chemical did you use to precipitate your gold out with (SMB)?
Cementing with copper will drop gold, and other things in solution that are less reactive like Ag, Pd, and Pt. It also drops a lot of copper so that black sand will have to be refined.

Crucial to know if your nitric solutions is still testing positive for gold. If so, go to the hardware store and buy some sulfamic acid crystals. Read the label carefully it must be pure sulfamic acid. I find it at Lowe's and Home Depot. Take a small amount of each of your solutions, and try a pinch in each. Then drop with SMB (Bonide Stump Remover only Home Depot carries it here).

I have to re-read your posts, and stand to be corrected. Excess Nitric will keep gold (and others) in solution, which is why de-noxxing with sulfamic is a step often overlooked. Very common to want to drive the reaction along faster by adding more Nitric, but it must be neutralized before trying to drop the gold.

Lastly there is a technique for suspending the copper plate in solution for cementing, I have not mastered this yet.

I hope this helps your situation.

 

[Hartbar]

I think thats a pretty solid idea.
But, one or two things that are sticking out to me is -18k gold needs inquarted so it doesnt cause problems... like, not allowing nitric to dissolve constituents. If one of those is silver, then you will make a silver chloride crust when you are attempting AR. But, you can gamble and may get lucky and have no silver in its alloy.

When you say "bands" did you just throw the whole thing in there? Or did you tediously separate the caps off of each link on the band?

Gold got in your solution from some free chlorine somewhere in the process. Probably the water you used to dilute the nitric. Chlorine is everywhere, really
Its probably very little gold in there. Leave the copper to cement it out. Then go from there.

The silver chloride crust happened to me recently, how do you fix the problem. I’ve got about 8 pieces of metal that would not dissolve in AR

 

[Topher_osAUrus]

The silver chloride crust happened to me recently, how do you fix the problem. I’ve got about 8 pieces of metal that would not dissolve in AR

Well, when i had a good part of a class ring, I just hit it with a hammer a few times then tried redissolving. Then recovering the AgCl as usual after rinsing.

 

[ZiegenSauger]

Thank you, guys! Much appreciated indeed.

@1mysurveymail:
You are correct, BLUE solution is Stannous negative for anything. I used Copper sheets and recovered 15 g of cement Silver approximately. I did not de-nnox this one since I was absolutely sure I have consumed all HNO3 since I go in increments ... I was wrong. The only bad thing is the unnecessary consumption of extra Copper.
BTW, I have Sulfamic acid, Urea, etc.
The GREEN solution was positive for gold, this one had consumed all HNO3, the Copper sheets came out about the same width and thickness, the picture shows the approx. 5-10 g of cemented whatever.

The AR yielded me 4.5 g of twice refined Gold. What a surprise surpassed my calculation and, consider scrap cost, material use, and time, this is profit. I have 15 g of gold, which I will make into a bar or ball (I am VERY BAD at pouring, even though I have poured two dozens ~4Ozt Silver bars, only 3 of those were seamless poured, the other either I had to remelt or to accept whatever ugly Frankenstein monster it looked like).

I tried to pour gold once ... did not go well. Possibly I will melt and leave it be whatever format in the bottom of the crucible.

Now my catch 22 situation: I have everything in the pictures plus the filtered papers and particles and a couple of caps I dropped on the floor everything incinerated. It is so little, but my curiosity is killing me. I am doing good recovering whatever has > 0.7 g of Gold.

I have a 4 x 4 x 1 inch Tupperware full of gold solution wipes, AR filter papers. Rationally it would be it the gold refiners constitution Article III: accumulate a decent amount of leftovers to try to recover something, otherwise, it will be a potential waste of time and products.

I should do this, but my curiosity is INSANE to find out whether that stuff from Nitric is indeed Gold.

Anyway, I've read hundreds of posts in the forum, many of them several times to go back to stubbornness and stupidity. I am going to incinerate the bulk of the Gold refining leftovers and add to this little bunch. Whatever Gold I recover we'll be from all that.

Butcher and a few others had handed my butt back to me in ashtrays :shock: :lol: :lol: one too many times already

 

[butcher]

Do some research on roasting, and the volatility of acids and salts, chloride salts as well as other halide salts which can make our values or metals go up in smoke, a little study can help you keep your gold or silver.

For example silver salts fused in sodium carbonate can help to keep your silver from going up in smoke...

For example adding a little sulfuric acid (or adding dry sulfate salt or ore) to wet materials containing chloride salts, begin heat low allowing nitrates and chlorides to form gases, the very small amount of the less volatile sulfuric will help to drive off the more volatile components of the metal salts, converting water, nitrates and chlorides to gases.

Very slowly raising heat will help to keep your values from becoming volatile and going up in smoke.

As salts begin to remove more volatile components the salts will begin to fuse.
Raising the temperature of your fused salts with stirring allowing them to evaporate, only as much as possible without forming large bubble of popping syrup and splashing as they burst at surface, lower heat if needed or give gas a way to escape, raising heat to dry and convert salts.

At higher temperature may stay molten (and crystalize if cooled), bubbling of the off gases can become problematic, keeping a portion of the pan the salts are on free of salt with stirring allows the liquid salts from the pan with stirring allowing the volatile gases formed on the hot the bottom surface of the pan free to escape through the fused syrup of salts.
other ways or methods you can use to help solution from bubbling and popping as gases escape , you can add paper( which adds carbon which is a reducing agent for base metals, or add previously roasted materials to this batch to help disperse the unroasted salts in this batch giving gases n easy place to escape the molten syrup.
You can also use something like ground up glass shards or other suitable material (resistant to acids or could be used as flux,,,) to give the gases a place to escape.

As these salts are heated and the more volatile gases (acid salts turn to gases and escape) the fused syrup of salts will begin to dry making it easier to raise het without gases bursting or being a problem, raising heat can make some more molten and dry mass to balls or crust keeping these crushed to powder as heat is raised (cooling if necessary and crushing to powder and return to drying and roasting process), slowly raise the heat to a red glowing heat (heating the pan from bottom with the hot plate while directing a torch flame on the dry crushed salts, keeping the powders stirred in air or oxygen, the glowing red metal salts will drive off the less volatile sulfuric salts, these metal salts exposed to air or oxygen for a period of time will form oxides of base metals (removing the salts of the acids), roasting the material if done properly will keep your values from becoming volatile and going up in smoke with the gases converting the salts of metals to elemental metal or oxides of metals.

the roasted material your valuable metal or base metal oxides can be then be treated with most any method panning, or with wet chemistry using acids or in smelting processes or other...

 

[jadedalex]

Zeigen, 18 Karat gold is not "pure". Even 24 Karat isn't "pure" because it still has minute (mine-yoot) quantities of residual metals. The closest "pure" gold is 99.9995 Fine gold and even that is not technically pure. Perhaps, at the core of a Giant Neutron Star, would you find 100% pure Gold. Trying to get 6 nines or purer would cost you more than the Gold is worth...
That said, try your damdest of eliminate as many impurities from your PM batch. This will require several steps. The knowledge of how to do so with the process you are contemplating is available in the Library on this site. Read. then read again. then read until you KNOW that you can do the process. THEN, do the process SAFELY....Good Luck.

 

[ZiegenSauger]

The conclusion, at last.

I dropped "whatever" from the suspicious green Nitric treatment. I collected leftover solids from temp. containers and wipe papers. I incinerated all these until no smoke powder was left.
Grinded all to fine powder.
Nitric treatment.
Filter and wash.
A/R.
Positive Stannous for Gold.
Dropped with SMB.
Washed clean with several baths of water and HCL.
Refined with A/R and repeated above 3 steps all over.
Weighted.
Melted to egg-like shape.
Freaking 5.3g fellas. Insane surprise, even thought it makes sense because of the relative volume that dropped from the green solution and the wipes being mostly from an old boiled over A/R, even though I am happy.

Thank you @butcher (as always) for the advice on roasting and volatility. Have compiled a couple of articles. Did not find anything specific in the forum yet but I need to fine tune my search.

Thank you for the tip @jadedalex. I am good on purity though. I have been very successful with Silver and no more mistakes with Gold. Even some misteps I am being succesful to correct path.

My goal for this year is 3 Ozt. I have a 15.xx gram bar, a 5.xx gram egg, a 9 gram blob, and 3 batches (one from 530 gram watch band caps, one from my first full.stock pot solids, and one from watch internals).

I will beat 1 OzT for certain. Now I am going to "prospect" on eBay and yard sales to try to meet my goal..

I am so happy. Even revovered from errors and mistakes. I had 8 buckets of shame accumulated from those.

Now, 52.5 OzT of Silver and 21g of gold later, I am in the right path.

Cheers

 

[ZiegenSauger]

Since I started this thread with wrist watch bands, I did an experiment with the first batch I mentioned at the top that yielded me a few grams of gold.
Now, in parallel with the procedures mentioned here, I had the opportunity to repeat the experiment, this time with purpose, annotating in my journal and paying attention to numbers and measurements.

As intro., I found a reliable source of gold filled watches (old, scrap, discarded). This second time, I acquired 530 g of "raw" material. Then I proceeded to sort it out: the main pile consisted of the band caps, the watch cases and, when possible, the watches internal gold gears.
I re-assured all items were stamped 10k 1/20 GF.
The second pile consisted of the bottoms, chains, links, flats and the actual watch assembly.
The last pile consisted of whatever I considered trash like coils, connecting bands, fillings, pins, poles, the metallic linking where bottom and top caps are mounted upon, etc.

The first pile is where I extract gold from: from the 530 g total, I got 238 g of usable material, my estimation is 0.025 x weight in usable material. I predicted something around 12g and got 12.3 g.

Now for the second pile of about 170g of what should be mostly iron (stainless steel, some brass, some nickel).
I immersed on some of my recycle A/P reactivated with Copper II Chloride (sorry if mispelled), in shaker table and light heat.

After filtering and washing, the leftover mud went directly to some of my leftover diluted nitric on heat. After no more reaction is present, filtered and washed (leftover over mud had iron rust color with some more tangerine fruit accent).

Rare earth magnet to retrieve every last bit of magnetic pieces. Then to AR. Recovered further 3g of gold.

Not sure yet if the extra time, chemicals, processing, mess (even though I mostly reused not fully consumed chemicals from previous processing), for me, someone who is struggling to reach 3 Ozt of gold by the end of the year, maybe as a hobbyist it is worth my while.

 

[FrugalRefiner]

ZiegenSauger, thanks for sharing your yield data. That's very generous of you.

Dave