Nitric nightmare - gold filled, help please

[Topher_osAUrus]

Sweet! lol, well at least I have all the tin I could ever need =P the tin must be what looked like lead to me when I clipped the jewelry open? was a metalic grey color easy to cut through after the outer shell. The gold metal on the outside flaked off the outside pretty easy as well after I clipped it.
Use that as a clue next time. (I'm sure you would have anyways, without me mentioning it!) Sure, the soft metal could have been silver, but 'the gold flaking off instead of being a solid shell.' -That is a dead giveaway. However, I should mention, that goldfill can be worn very very thin, and itself(gold layer) does get worn thin to the point of it being nothing but flakes (after dissolve, though)

Thank you for being so awesome Topher!
Alright, when I get home I'll filter (im thinking I'll syphon and filter all of the emerald solution off of the top to get mostly "tin free" solution and also all of the floating at least gold colored metal out before filtering the tin sludge, grab the low hanging fruit so to speak.)
I, personally, would keep,it all together. Instead of making one process into two (which in turn would end up being like ten...after processing the small flakes, the other stuff would get done to a point where you are running the same processes, and in the end,
the waste is doubled up -maybe even tripled)
Then after filtering, rinse the solids with distilled water, and let dry. Would drying them in the coffee filters in a large bowl crucible in a kiln be advisable to speed up the process? maybe 200F? or just dry them in a pyrex dish on a hot plate? (I have sand in the hot plate to disperse the heat to avoid cracking, seems to work well even when dry.)
Well, yes filters are good and bad in this case, one they will help speed up the drying process, but 2, after they are burnt the carbon can/will reduce some metal salts. This could reduce your tin back to metal, in this case, we are wanting to oxidize the tin.I would say having the filters would not do much harm, as the tin will oxidize anyways (with good stirring and access to air).

You should slowly dry the mess though, once most of the moisture is gone, slowly start raising the heat, it will eventually turn into a syrupy mess, then start to dry out again. Just keep stirring it throughout the process and eventually bring it to red heat with stirring. I would opt for a torch instead of kiln though. Butcher explains the incineration process MUCH better than me. Do a search for "incineration" with "butcher" as the author [omit the quotations]
Does the torch matter? I have Oxy & acetylene, oxy & propane, just propane and MAPP torches, not sure how fine the solids will be and if one torch might get too hot and melt instead of heat or may blow the solids away (and I have made enough mistakes so I thought I'd ask =P)
I would go for whichever one has the most timid flame. When Im drying and roasting tin sludge, most of the work is done by my hotplate, only finishing up the process do I use my torch.

And then throw it all into a pyrex container with HCL (should I dilute the HCL with distilled? and if so how diluted? or do I want to avoid water and oxygenating the HCL?)
I use full strength 30%, but that doesn't mean I'm right, or that is the only strength that can be used.
PS. Topher, I have had many professional lives, Electrical engineer, IT architect, Vet tech, Network engineer and even a mechanic... I can and will learn as quickly as I can, since I have found this forum I have been reading chunks everyday, I hope to become an asset to this forum eventually instead of a burden.
Just paying it forward best I can. This forum and its members are a godsend.
And I sincerely want to thank you for your patience, positive attitude, knowledge and experience! Thank you good sir! If you need any IT, Electrical, Mechanical or Animal advice =P let me know!

Thank you kindly, hopefully you get some gold out of this endeavor!

 

[ImTechMan]

Thank you kindly, hopefully you get some gold out of this endeavor!

Thank you! me as well! =P Should I try to salvage the 1.5 liters of nitric? it is so saturated with unknown base metals I wouldn't even know where to start. So I will start by searching the forum! =P (I will obviously take your previous recommendation and try to cement out any silver with copper, unless that recommendation has changed with the addition of the sulfuric, but since pure-ish sulfuric is used in the de-electroplating cell I am assuming it will be fine, I'll of course research it first for safety.)

Also on a side note, the dark green solution goes brown with stannous chloride, something else for me to research!

 

[Topher_osAUrus]

Thank you kindly, hopefully you get some gold out of this endeavor!

Thank you! me as well! =P Should I try to salvage the 1.5 liters of nitric? it is so saturated with unknown base metals I wouldn't even know where to start. So I will start by searching the forum! =P (I will obviously take your previous recommendation and try to cement out any silver with copper, unless that recommendation has changed with the addition of the sulfuric, but since pure-ish sulfuric is used in the de-electroplating cell I am assuming it will be fine, I'll of course research it first for safety.)

Also on a side note, the dark green solution goes brown with stannous chloride, something else for me to research!

Well, if you want to reuse the nitric (assuming there is free nitric left). You can test for silver in solution without sticking in copper (which would consume any free nitric left)
--
Take a few mL of solution, and to it add a few drops of HCl, or salt water. Silver nitrate will scavenge the chlorides and turn into silver chloride. If its positive, it will have a milky white to cottage cheese-ish precipitate form.
If the test is positive, you have a couple routes you can take to reclaim the silver.
-we will cross that bridge if we need to

Take another small sample, add a known weight of copper to it, add heat, let it dissolve all it will. Then take out, wash, dry and weigh the copper. Some math will tell you what the bulk of acid can still dissolve. If there is silver in solution, it will cement out from being displaced by copper. So this test could be substituted for the first suggestion, and the silver chloride avoided all together. If any Pd is in solution, it would get disppaced by the copper as well.

If you think the green solution is testing positive for palladium, a Dimethylglyoxime test will give a definitive answer. I would be surprised if it had Pd in it though. The green is probably from free acid, or dissolved iron, or both. The brown test result is probably a false positive. I could be wrong though, it would not be the first time.

 

[g_axelsson]

Thank you kindly, hopefully you get some gold out of this endeavor!

Thank you! me as well! =P Should I try to salvage the 1.5 liters of nitric? it is so saturated with unknown base metals I wouldn't even know where to start. So I will start by searching the forum! =P (I will obviously take your previous recommendation and try to cement out any silver with copper, unless that recommendation has changed with the addition of the sulfuric, but since pure-ish sulfuric is used in the de-electroplating cell I am assuming it will be fine, I'll of course research it first for safety.)

Also on a side note, the dark green solution goes brown with stannous chloride, something else for me to research!

I just want to remind you two that silver sulfate isn't very soluble in cold water. Only 8 g per liter.
http://goldrefiningwiki.com/mediawiki/index.php/Silver_sulfate
That is the reason that we usually recommend using nitric acid free from sulfates when working with silver.

Göran

 

[Topher_osAUrus]

I just want to remind you two that silver sulfate isn't very soluble in cold water. Only 8 g per liter.
http://goldrefiningwiki.com/mediawiki/index.php/Silver_sulfate
That is the reason that we usually recommend using nitric acid free from sulfates when working with silver.

Göran

Ah, yes.
I did have a brain fart on that one.

Do you think, if lead and silver were in solution, and a small amount of sulfuric were added, that both would be converted to their sulfates? Or would lead be preferred over silver? (Assuming most sulfuric didnt get consumed when making the iron go into solution)

Now Im curious!
What happens?!?

Ferrous sulfate, then lead sulfate, then silver sulfate?
-im going to have to dig into my silver book again, but I know ferrous sulfate reduces silver sulfate. But, that is using the products from 2 different reactions. Not in a mix of competing complex reactions. Which im sure complicates things greatly.

Edit to fix continuity

 

[g_axelsson]

Do you think, if lead and silver were in solution, and a small amount of sulfuric were added, that both would be converted to their sulfates? Or would lead be preferred over silver? (Assuming most sulfuric didnt get consumed when making the iron go into solution)

I would assume that any dissolved silver sulfate mixed with lead in solution would form lead sulfate and whatever silver and the other ions would do (lead chloride for example would lead (no pun intended) to silver chloride precipitating at the same time). Any precipitated silver sulfate could then dissolve and react with more lead but it would probably be quite slow as any silver sulfate crystal would get a coating of insoluble lead sulfate.

This is purely theoretically though, and nothing I have tried or planning to try.

Göran

 

[Topher_osAUrus]

I would assume that any dissolved silver sulfate mixed with lead in solution would form lead sulfate and whatever silver and the other ions would do (lead chloride for example would lead (no pun intended) to silver chloride precipitating at the same time). Any precipitated silver sulfate could then dissolve and react with more lead but it would probably be quite slow as any silver sulfate crystal would get a coating of insoluble lead sulfate.

This is purely theoretically though, and nothing I have tried or planning to try.

Göran

It would have been silver nitrate though, (in his case - but, I do see where you are coming from, and agree [theoretically] completely )

So the sulfuric added to that (hypothetical) silver nitrate and rust and lead nitrate mix. Probably would have made some silver sulfate, lead sulfate, and ferrous sulfate. But would the copperas dissolved in the messy solution be oxidized the ferric sulfate and reduce the silver back to metal... Hmm. :?
I dont know... And I dont think I want to go make a mess just to find out!

 

[goldsilverpro]

What does "tested" gold filled mean??? If it was worn jewelry, every piece would run different, no matter what it is marked.