# Guys I screwed up...



## Goldman94 (Apr 9, 2020)

I'm just gunna start by saying, please dont roast me and please just help fix what I did. I would really really appreciate it...

So I added probably about 1/4 cup of baking soda to my AR mix to denox the nitric, which I know was a bad idea now. What can I do now? I'm stuck here guys, please help


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## Lou (Apr 9, 2020)

Evaporate and reconstitute in HCl. Then invest in sulfamic.


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## Goldman94 (Apr 9, 2020)

Lou said:


> Evaporate and reconstitute in HCl. Then invest in sulfamic.



What's this thing about cementing with copper too? I see that people do that as well. Do I have to do that? Or can I just evaporate and add more HCL?


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## anachronism (Apr 10, 2020)

Goldman94 said:


> Lou said:
> 
> 
> > Evaporate and reconstitute in HCl. Then invest in sulfamic.
> ...



Compared to using Sulphamic and something like SMB, cementing with copper is slow and laborious. Adding HCl and evaporating is what you would be told to do 100 years ago- Sulphamic is the modern, up to date version.


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## butcher (Apr 10, 2020)

Sodium hydroxide NaOH will not effectively deNOx aqua regia gold solution, although it will convert the acids to salts.

Sodium hydroxide and hydrochloric acid form a salt, we often call table salts NaCl and water.
HCL + NaOH --> NaCl + H2O

Sodium hydroxide and nitric acid form a salt of sodium nitrate.
HNO3 + NaOH --> NaNO3 + H2O

Aqua regia and sodium hydroxide would produce salts of both NaCl and NaNO3 and water, once evaporated if gold or base metals were involved in these salts later additions of HCl would reform aqua regia (poor-mans) and put the base metals and gold back into solution...

Base metals in a solution like copper would form salts with lower oxidation states CuCl or form oxides CuO and hydroxide salts Cu(OH)3 of the base metals with the sodium hydroxide depending on concentrations...
CuCl2 + NaOH --> NaCl + Cu(OH)3

Base metals forming like CuCl forming would begin to bring gold out of solution even before these base metals formed hydroxides of the metals.
AuCl3 + 3CuCl --> Au + 3CuCl2

Sodium hydroxide will also precipitate gold as a hydroxide.
AuCl3 + 3NaOH --> Au(OH)3 + 3NaCl

Excess of hydroxide can the amphoteric metals back into solution.

With an excess of sodium hydroxide, the gold can be redissolved back into the liquid solution as a soluble sodium gold hydroxide solution.

Au(OH)3 (s) + NaOH --> NaAuO2 (aq)

With gentle heat, the base metal hydroxides can form base metal oxides, around 500 deg the gold hydroxide will decompose to gold and oxygen (Higher heat can put gold into vapors with the chloride salts losing gold in the smoke).

Au(OH)3 --> Au2O3
Au2O3 --> Au + O2 (reaction not balanced)

Now we have the solution evaporated the water and the acids converted to salts like NaCl, NaNO3, CuCl, Cu(OH)2, Au(OH)3, adding HCl at this point can put gold back into the newly formed poor-mans aqua regia...

NaCl + NaNO3 + HCl + Au(OH)3 --> gold dissolved back into the poormans aqua regia along with the other base metals in solution ...

So here your back to having an aqua regia solution that may need to be DeNOxed to recover your gold...


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## anachronism (Apr 10, 2020)

butcher said:


> Excess of hydroxide can the amphoteric metals back into solution.



Yoda? 8) 8) 8)


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## goldenchild (Apr 10, 2020)

Are you just looking to get your gold out of solution? If so why not just add HCL until the solution is acidic again? It shouldn't take much. Then proceed as normal.

ETA: Urea also works well to get rid of nitric


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## Goldman94 (Apr 10, 2020)

goldenchild said:


> Are you just looking to get your gold out of solution? If so why not just add HCL until the solution is acidic again? It shouldn't take much. Then proceed as normal.
> 
> ETA: Urea also works well to get rid of nitric



I tried but the SMB just wouldn't work. I am currently reducing the solution to a syrup and will then add in more HCL then SMB in hopes of then precipitating the gold. 

If that doesn't work, what should I do next?
And if it does work should I redo everything to clean it up some more or would it still be in its purebred state?

Thank you guys for all the help, I really appreciate it


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## Goldman94 (Apr 10, 2020)

So this is my current situation...

After reducing down the solutions to a syrup consistency I added in some HCL then some SMB and this is currently what it looks like. I have no idea why one is yellow and the other is brown. They were both like that before this and and both has baking soda in them...

I would really love to just start all over but I'm lost now
There should be about 9 grams of gold in there between the 2 so I really can't afford to lose it


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## galenrog (Apr 10, 2020)

You may have already done this, but you did not mention it. Did you test your solution for gold?

Time for more coffee.


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## Goldman94 (Apr 10, 2020)

galenrog said:


> You may have already done this, but you did not mention it. Did you test your solution for gold?
> 
> Time for more coffee.



I just tested it and it was positive in the yellow one. Not so much, if any in the brown one. I'm confused. In both it seems like some metallic gold may have precipitated out somehow too.


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## anachronism (Apr 10, 2020)

Please show us a picture of the test.


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## Goldman94 (Apr 10, 2020)

anachronism said:


> Please show us a picture of the test.



The yellow solution turned brown/purple instantly and the brown solution had almost no change to the stannous.

Here's some updated pictures as well. It does look like theres some brown powder on the bottom of both along with some gold metallic flakes. 

I also decanted off some of the yellow clear solution into another beaker with hopes of using SMB to precipitate but all that happened was a bunch of fizzing and nothing came out.


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## butcher (Apr 10, 2020)

Testing may not show gold in all of its different oxidation states, it will not detect reduced gold...


anachronism said:


> butcher said:
> 
> 
> > Excess of hydroxide can the amphoteric metals back into solution.
> ...



Sorry for the confusion, I forgot to put the word put into that sentence.



Excess of sodium hydroxide can put the amphoteric metals back into solution.

Many metals will precipitate from a solution when a basic solution like sodium hydroxide is added, the amphoteric metals will redissolve back into solution if you add an excess of a basic solution (in this case caustic soda), you can precipitate gold and then if not careful you can re-dissolve it back into solution with an excess of sodium hydroxide...

Gold can be precipitated with the use of NaOH, using an excess NaOH will redissolve gold back into solution...
https://en.wikipedia.org/wiki/Amphoterism


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## Goldman94 (Apr 10, 2020)

butcher said:


> Testing may not show gold in all of its different oxidation states, it will not detect reduced gold...
> 
> 
> anachronism said:
> ...



What do you suggest I do then? I have so much contamination in there I have no idea what to do next. Theres a thick layer of baking soda in there along with probably some undisolved SMB and paper from the filter that I tried to dissolve when I made the AR, since the first time I did it I wasnt happy with the debris that came thru the paper as well as how much yellow AR solution was still in the paper.


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## butcher (Apr 10, 2020)

Lou said:


> Evaporate and reconstitute in HCl. Then invest in sulfamic.


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## anachronism (Apr 10, 2020)

No worries butcher I was smiling with you not at you. Its hard when you crack off a fast informed post.


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## Goldman94 (Apr 10, 2020)

butcher said:


> Lou said:
> 
> 
> > Evaporate and reconstitute in HCl. Then invest in sulfamic.



I tried that and nothing happened...except for the sulfamic part. What happens to the baking soda layer? That's probably an inch or 2 thick. And I should add the sulfamic instead of the SMB?


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## butcher (Apr 10, 2020)

After evaporating the solution, adding HCl will dissolve the salts back into solution, any excess sodium hydroxide will dissolve with the HCl forming a sodium chloride solution, along with the other metals also dissolving as chlorides.

This may or may not put your gold back into solution ---depending on how much nitric was formerly involved or how much sodium nitrate salts are involved in the mix of salts...

When adding HCl to the evaporated salts, I would add just a little acid at first, to form a very concentrated syrup-like solution, taking note if any brown gas is formed, indicating NOx gases being produced from the acidic HCl and possible nitrate salts reacting.

Evaporate the solution again to almost syrup, add just a little HCl to rewet and take note of any gases formed...

Evaporate the solution for the third time...

If you invested in sulfamic you could avoid some of the evaporation steps here...

Depending on circumstances everything may not dissolve, back into the concentrated solution as you added the small additions of HCl, some gold may have dissolved into the syrup and some gold foils may remain...

If everything did dissolve back into solution as you finished your third evaporation to a syrup consistency, then you could just add water as suggested in Hoke's and continue as instructed.

Personally I would prefer everything was back into the solution before proceeding, including gold if it did not all go back into the solution I would put it back into solution with controlled additions of nitric along with HCl as needed...


If your still lost, sit this mess aside and then Read Hoke's book...


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## Goldman94 (Apr 10, 2020)

butcher said:


> After evaporating the solution, adding HCl will dissolve the salts back into solution, any excess sodium hydroxide will dissolve with the HCl forming a sodium chloride solution, along with the other metals also dissolving as chlorides.
> 
> This may or may not put your gold back into solution ---depending on how much nitric was formerly involved or how much sodium nitrate salts are involved in the mix of salts...
> 
> ...



I dont know how much of a difference there is between the 2 but I used sodium bicarbonate (baking soda) not hydroxide


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## galenrog (Apr 10, 2020)

Where did sodium hydroxide come into the conversation? I read in the original post that he added sodium bicarbonate (baking soda). Did I miss something?


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## Goldman94 (Apr 10, 2020)

galenrog said:


> Where did sodium hydroxide come into the conversation? I read in the original post that he added sodium bicarbonate (baking soda). Did I miss something?



Yes you're right, it was bicarbonate not hydroxide.


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## butcher (Apr 10, 2020)

I may have been the cause for this discussion going from a base like sodium bicarbonate being discussed instead of a base like sodium hydroxide being discussed, I do not know if my old age will hold up as an excuse or not. Or if I just misread the base goldman94 used originally...

Most everything still holds relevant in this discussion, and most of all the reactions are similar except maybe for some CO2 gas evolution along the way that using the caustic NaOH would not have formed...

Sodium hydroxide and hydrochloric acid form a salt, we often call table salts NaCl and water.
HCL + NaOH --> NaCl + H2O

Sodium bicarbonate and hydrochloric acid form a salt, we often call table salts NaCl and water with the evolution of CO2 gas.
HCl + NaHCO3 --> NaCl + H2O + CO2

Sodium hydroxide and nitric acid form a salt of sodium nitrate and water.
HNO3 + NaOH --> NaNO3 + H2O

Sodium bicarbonate and nitric acid form a salt of sodium nitrate in water with the evolution of CO2 gas.
HNO3 + NaHCO3 --> NaNO3 +H2O + CO2

About the only difference besides CO2 gas emission, the only other point I can see different is that with the bicarbonate not being as basic as sodium hydroxide is. you are not likely to get the amphoteric gold to dissolve as a base with an excess of sodium bicarbonate...


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## Goldman94 (Apr 10, 2020)

butcher said:


> I may have been the cause for this discussion going from a base like sodium bicarbonate being discussed instead of a base like sodium hydroxide being discussed, I do not know if my old age will hold up as an excuse or not. Or if I just misread the base goldman94 used originally...
> 
> Most everything still holds relevant in this discussion, and most of all the reactions are similar except maybe for some CO2 gas evolution along the way that using the caustic NaOH would not have formed...
> 
> ...



First of all, I just want to immensely thank you for everything that you've done for this thread and the forum in general, you really know your stuff. 

As to what to do next, what you're suggesting to me is that I should evaporate my solution/salts mixture until syrupy and then add in HCL and repeat a few times? Then after that should all the salts be gone by then? And then I can just precipitate the gold out then? Do I need to use anymore nitric in this?


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## butcher (Apr 10, 2020)

Goldman94,

Sorry if I am complicating things for you, it is not my intention.


You could do this in a few different ways and still come up with the same results.

you can just evaporate the liquid and as suggested, or just test the solution for gold if it test shows violet in the reaction with stannous chloride you have gold in solution, if it is brown it is likely a false positive (if you previously used SMB or some other sulfite)...

If tin was involved you could even have invisible to the eye gold floating in solution as colloids that will not show up in a stannous chloride test...

You can decide for yourself if you wish to trust the test and treat the solution for waste or evaporate it to concentrate it and treat it along with the salts you have now.

If evaporating the solution, I would separate the salts you have now from the liquid while evaporating the liquid to concentrate it, you can add it back to the salts you have now after the water is removed before reconstituting in HCl...
--------------------------------------------------

Now you should be left with salts (and possibly a very concentrated liquid).
Here we can add some heat and just a tiny bit of HCl.

Just as it describes in Hoke's book.

Any nitrates in solution (or salts) once acidified by adding HCl. will reform nitric acid, in the heat of this concentrated solution, they will also convert to gases, evolving a red-brown cloud of deadly gaseous NOx.

Here we again evaporate to remove water, to concentrate and to help decompose nitrates and remove nitric as gases(evaporate water which came from the added HCl we added, which is 20% acid and 80%water, and any water created in the reaction, along with any nitric created in the reaction).

Repeating with another small addition of HCl to the concentrate (watching for the deadly gas to evolve indicating nitric or nitrates remaining)...

Repeat the third time to insure decomposition of any nitric or nitrates...

Now we still have a concentrated saturated chloride solution of salts free of nitrates or nitric.

if you did not have a tin in solution with the gold originally I would proceed.
Bringing the salts back into solution with HCl...
-----------

a test to check for possibly problems with tin would be to see how well the solution filters before you concentrating it, if it will not pass the filter easily I would suspect tin is involved and go ahead and dry the salts, fuse them, and roast them)...

if tin was originally involved with the gold in solution, I would consider a possibly fusion of the salts to oxidize and tin salts that may be involved) in this case dry everything to salt at low heat and then heat the salts (keeping them stirred while they evolve gases, heating the dried salts until they melt into a thick syrup, then keep heating until this syrup dries to a crust, crushing the crust to powder and roasting the powder to a red hot glow, cool crush again and reconstitute in HCl...


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## Goldman94 (Apr 10, 2020)

butcher said:


> Goldman94,
> 
> Sorry if I am complicating things for you, it is not my intention.
> 
> ...



Okay, so what I should plan to do is decant as much clear liquid off as I can from the beakers and evaporate that down and reconstitute with HCL then precipitate out with SMB? 

As for the salts, I'm still kind of confused as to how to recover the gold from them. It is a very thick layer of gunk at the bottom along with some brown powder and what looks to be metallic gold. 

As I mentioned before, there should be about 9g of gold in there and I cant afford to throw out any solution or salts that may contain the gold in them.


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## anachronism (Apr 10, 2020)

Richard

A Chemistry question. If as you say the gold is in a hydrous form then shouldn't HCl alone then convert it back to the Gold Chloride?


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## denim (Apr 10, 2020)

Goldman94 said:


> As I mentioned before, there should be about 9g of gold in there and I cant afford to throw out any solution or salts that may contain the gold in them.



Sorry if I missed something already mentioned but is the amount of solution shown in the two beakers all the solution you have? The yellow solution certainly looks like it could have some gold in it but not 9 grams. My experience, which is minimal, would suggest that 9g of gold in 200ml of solution would be more of an orange color. The other darker solution might have some gold in it but you said it's test came back negative. What, and how much of it, was the source material?

Dennis


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## Goldman94 (Apr 10, 2020)

denim said:


> Goldman94 said:
> 
> 
> > As I mentioned before, there should be about 9g of gold in there and I cant afford to throw out any solution or salts that may contain the gold in them.
> ...



I had 18g of 10k and 4g of 14k which should equal 9.8g of 24k.

Yes that is all the solution I have. I was confused as to the color difference between both of them too. It started as a very dark orange color and then when I added the SMB nothing came out and then I decided to add baking soda to neutalize the nitric, but now I know that was a very bad idea. So after adding that it turned the color to a bright yellow and the other, darker, solution stayed the same. 

As I mentioned before, i think some of the gold has already precipitated out due to a brown mud at the bottom, along with some metallic pieces that look like gold. 

This is why I'm very confused since the first time I did it I had 0 issues with it but the next time I have no idea what I did wrong. I have a feeling that some gold is still in solution but the majority of it is trapped inside the sediment at the bottom and have no idea on how to retrieve it.

But I do have a feeling i lost a lot of gold and I have no idea where it could have gone...


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## Goldman94 (Apr 10, 2020)

This is what I'm left with now. I'm currently trying to evaporate the solution on the burner and the other one is just all the sediment I have that I believe has the majority of gold in it. Since the one I have on the burner tested negative for any gold in solution I'm confused since I combined all the solution in that one and all the sediment in the other one.


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## butcher (Apr 10, 2020)

I have a bad habit of posting then editing and reposting, or thinking of something to add to the post, and edit, normally it is not a problem as nobody has time to post or post before I finish.

Here you guys are reading and posting before I finish editing, and even quoting, making my bad habit obvious and a problem, no wonder editing posts is discouraged by the forum rules.

Jon, I cannot answer that, I do not know from experience if Au(OH)3 is soluble in HCl alone or not.


https://en.wikipedia.org/wiki/Gold(III)_hydroxide
https://chemequations.com/en/?s=Au%28OH%293+%2B+HCl+%3D+AuCl3+%2B+H2O

I would expect he does not have a gold hydroxide, but the base metals involved in solution has most likely reduced his gold as they formed oxides and hydroxides as metallic gold, I doubt the baking soda could even form a gold hydroxide like NaOH can


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## Goldman94 (Apr 10, 2020)

Theres definitely metallic gold in here and a brown powder. Should I just pan it out? Lol


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## butcher (Apr 11, 2020)

That is an awful lot of salts.

I am just curious, have you tested the pH of the solution?
Either way acidic or basic it still holds metals in solution, I am doubtful it would hold any gold, it would most likely have precipitated as black powder long ago from the base metals in solution (and as salts now).


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## Goldman94 (Apr 11, 2020)

butcher said:


> That is an awful lot of salts.
> 
> I am just curious, have you tested the pH of the solution?
> Either way acidic or basic it still holds metals in solution, I am doubtful it would hold any gold, it would most likely have precipitated as black powder long ago from the base metals in solution (and as salts now).



I have not checked it, I dont have a ph kit but I would assume it is very acidic from when I was adding in baking soda last night it continued to fizz like crazy.

I think we may be getting somewhere though, I have no idea how but I've been seeing quite a lot of metallic gold being separated out somehow, as well as brown powder that is mixed in with the salts. I have a feeling much more is mixed in there but I just cannot see it. 

I'm still trying to figure out a way as to how I can separate the gold from the salts, as well as if any of the salts contain gold that need to be chemically extracted, that part is where I will be stuck longest.


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## Goldman94 (Apr 11, 2020)

Goldman94 said:


> butcher said:
> 
> 
> > That is an awful lot of salts.
> ...


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## Shark (Apr 11, 2020)

Are these salts soluble in water? I have never had sodium bicarbonate in my solutions before so I am not sure.


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## Goldman94 (Apr 11, 2020)

Shark said:


> Are these salts soluble in water? I have never had sodium bicarbonate in my solutions before so I am not sure.



Hmm, I may have to try that...


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## butcher (Apr 11, 2020)

Most of the salts will be water-soluble and dissolve in water.
HCl is around 80% water 20%acid.

If tin is involved, the tin hydrolyzes in water to gooey gunky SnCl4, where HCl will dissolve it better as SNCl2.
Thus HCl is suggested it will dissolve the salts, it has plenty of water, and the acid will assist to dissolve some of the salts that may not be as water-soluble now, also using HCl may save somewhat on the volume of waste that will be generated trying to clean this mess up.

If tin is not involved, and you do not mind evaporating more water from your waste stream later then I would definitely use water at first to dissolve as much of the salts as possible, before using acids...

A clue if tin is involved now would be to take a small sample a few milliliters of concentrated solution dilute it with water and see how well it passes the filter.

If the filter clogs or runs slow I would suspect tin is involved, and avoid using water at first to dissolve the bulk of salts, using HCl at least at the beginning to put the tin in solution.

Karat gold normally does not have a problem with tin (as long as solder is not involved) that gold-filled junk jewelry or electronic scrap has.

I do not know if any junk jewelry or gold fill is involved here in this batch unless each piece was tested before dissolving to verify that the karat marking was correct and the ring was not a fake, or gold-filled...


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## Goldman94 (Apr 11, 2020)

butcher said:


> Most of the salts will be water-soluble and dissolve in water.
> HCl is around 80% water 20%acid.
> 
> If tin is involved, the tin hydrolyzes in water to gooey gunky SnCl4, where HCl will dissolve it better as SNCl2.
> ...



What if I still have gold in solution? I'm not going to evaporate that off, am I? Also, no tin should have been present as everything was tested to be at least 10k and real karat gold.

By dissolving the salts, will the gold be precipitated out of the solution by itself or will it be in solution?

I'm going to try and adding water to it and evaporating it today like you said. Probably going to take quite awhile but hey, what can ya do.


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## goldenchild (Apr 11, 2020)

STOP. You're digging yourself into a bigger and bigger hole. At this point I think you should filter your solutions and put the liquids and solids to the side. If you go this route I can help you. If not your just going to keep spinning your wheels.


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## kurtak (Apr 11, 2020)

butcher said:


> Most of the salts will be water-soluble and dissolve in water.



:shock: --- that does not make sense - he has already "added" baking soda to his solution - enough baking soda that he precipitated carbonites/carbonates - which means he has raised the Ph (how much we don't know)

Simply adding (diluting) with water is not going to dissolve those salts - if anything it "may" allow more salts to fall out

until we know the PH of his solution after he added the baking soda we can't "fully" advise him on how to proceed

Depending on the Ph - I "might" just filter out the solids & then hit the filtered solids with HCl

From what I see - he has gold in those solids (how much we do not know) as the result of "first" adding SMB - then adding baking soda

When he added the baking soda - he may have (or not) killed most &/or all of the nitric - so depending on that - when he hits the solids with HCl - he may dissolve just the salts leaving the gold - or dissolve the salts & "some" gold (but leave some) - or dissolve both the salts & all the gold

Filtering out the solids "should" allow him to use less acid - why? --- because he only needs enough acid to dissolve the solids & NOT have to adjust the Ph of the solution "before" the HCl "starts" also dissolving the solids

The (filtered) solution --- need to know two things - what is the Ph - & what is the stannous test

From what I see - stannous shows a "trace" of gold - because it's a trace - again - I would want to know the Ph before I decided on how to recover that "trace" --- in other words - depending on Ph - do I need to lower the Ph to recover that trace - or can I recover it as is (&/or a couple other options I see with that solution)

In other words - I don't quite get why we are going around & around here without know what the Ph is as a result of his adding baking soda ?

Goldman94 - bottom line - if you are going to get into refining - besides having stannous in your tool box - you need to have a way to test Ph --- you don't need a Ph test "kit" &/or a Ph meter - but you at "least" need Ph test paper - you want the Ph test paper to be good for testing in the range from Ph 1 - Ph 13

if nothing else you need to be able to test Ph when you go to treat (adjust) your waste solution for "proper" disposal - can't just dump them down the drain - so get some Ph paper

Kurt


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## kurtak (Apr 11, 2020)

goldenchild said:


> STOP. You're digging yourself into a bigger and bigger hole. At this point I think you should filter your solutions and put the liquids and solids to the side. If you go this route I can help you. If not your just going to keep spinning your wheels.



:lol: :lol: :lol: 

The SHORT version posted before I posted :mrgreen: 

Kurt


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## Goldman94 (Apr 11, 2020)

Okay, so I just tested the solution with stannous and the results came back negative for gold. With all the sediment I see, it seems like a decent amount has precipitated out as gold flakes and a little brown powder (from what I see in the salts)

With how much baking soda I used, I believe I killed off all the nitric, since i only used about 10ml, but I cant be positive of that. 

As for the ph test, I'll go today and get one. What do I need to know about that? 

I think I will just filter off the clear yellow solution and keep the solids to the side. So keeping that to the side, should I add HCL until it's all gone?


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## Shark (Apr 11, 2020)

By adding the sodium bicarbonate, that would kill not just the nitric but the hydrochloric as well. 


As Kurt mentioned, you need to be able to test from Ph1 to Ph13. Swimming pool test paper won't go to the extreme high or low side, so they won't work for a full range of testing. I have a couple of digital PH meters that I got at a large nursery for testing soil acidity. They might not last long, but they can be bought for around $10. The one I like best of the two is made by Jellas, and I have been using it for over a year now. If you have a brewing shop near by they will sometimes carry a full line of Ph test papers and sometimes digital meters as well.


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## Goldman94 (Apr 11, 2020)

Shark said:


> By adding the sodium bicarbonate, that would kill not just the nitric but the hydrochloric as well.
> 
> 
> As Kurt mentioned, you need to be able to test from Ph1 to Ph13. Swimming pool test paper won't go to the extreme high or low side, so they won't work for a full range of testing. I have a couple of digital PH meters that I got at a large nursery for testing soil acidity. They might not last long, but they can be bought for around $10. The one I like best of the two is made by Jellas, and I have been using it for over a year now. If you have a brewing shop near by they will sometimes carry a full line of Ph test papers and sometimes digital meters as well.



I'm guessing I need a ph around 1? But if I just keep adding HCL and try to get rid of the baking soda by adding more and more HCL wont that work too?


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## FrugalRefiner (Apr 11, 2020)

You keep talking about treating all your solution or all your solids, but you have no idea what you have. When dealing with an unknow, the best tactic is to do some testing on SMALL amounts of each. When I say small, I mean test tube tests. So you would take a SMALL sample of your solids, put them in a test tube, then put in small amounts of HCL etc. to see what happens. When you find a method that works, then you can apply it to the rest of the batch.

You can buy wide range pH test papers on eBay for around a dollar.

Personally, I would advise you to set your mess aside and study. Reread this thread. Obviously there is a lot that has been said that you do not understand. Study till all the advice makes sense. Then when your pH papers arrive, you can pull your mess back out and proceed with some hope of getting your gold back out.

Dave


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## Goldman94 (Apr 11, 2020)

FrugalRefiner said:


> You keep talking about treating all your solution or all your solids, but you have no idea what you have. When dealing with an unknow, the best tactic is to do some testing on SMALL amounts of each. When I say small, I mean test tube tests. So you would take a SMALL sample of your solids, put them in a test tube, then put in small amounts of HCL etc. to see what happens. When you find a method that works, then you can apply it to the rest of the batch.
> 
> You can buy wide range pH test papers on eBay for around a dollar.
> 
> ...



It's not that I haven't studied any of this. I just made 1 costly mistake. If I never would have added the baking soda, I never would have been in this predicament.


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## Shark (Apr 11, 2020)

Goldman94 said:


> Shark said:
> 
> 
> > By adding the sodium bicarbonate, that would kill not just the nitric but the hydrochloric as well.
> ...



Don't guess. 

You have butcher, kurtack, goldenchild and Frugalrefiner, trying to guide you. Short of getting a full education in chemistry it don't get much better than than that.


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## Goldman94 (Apr 11, 2020)

I know, and they've been way more than helpful and I'm so grateful for all the knowledge that they've shared with me. 

I just want to get this mess figured out and recover this stupid gold


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## jimdoc (Apr 11, 2020)

Goldman94 said:


> I just want to get this mess figured out and recover this stupid gold



Gold is never stupid. Now tin, tin can get stupid.


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## Goldman94 (Apr 11, 2020)

jimdoc said:


> Goldman94 said:
> 
> 
> > I just want to get this mess figured out and recover this stupid gold
> ...



Lol...I'm just scared to see what my recovery will be when it comes to it. Im expecting close to 10g but I have a funny feeling it won't be close


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## butcher (Apr 11, 2020)

kurtak said:


> butcher said:
> 
> 
> > Most of the salts will be water-soluble and dissolve in water.
> ...


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## Goldman94 (Apr 11, 2020)

Little update...

Here's one of the beakers, this one had the most salts in it so I decided to put some water in there and it really dissolved a lot of the solids. I'm really curious as to what this powder is now. Theres a fine layer of metallic gold on the bottom that is covered in a brownish powder but it doesnt really look like gold powder. It does and doesn't, if that makes any sense. I'm really tempted to try and melt some of it down and actually find out whether or not it is gold powder. It has a very fine consistency to it but it settles very quick to the bottom.


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## butcher (Apr 11, 2020)

Don't melt any down at this point you could put your gold up in smoke and make it harder to get back.

It is doubtful the gold dissolved when you added water, but I would do a stannous test of the solution to confirm (I would also check pH and make sure it was at least somewhat acidic before doing a stannous test).

After decanting adding HCl, will begin to dissolve more of the salts, but also could put some gold in solution, that is if some of the salts are nitrates which may form a poor-mans aqua regia as you add HCl (so the stannous tests will be much more important to determine if the gold is being dissolved back with the salts and other base metals).

Basically, if water dissolves most of the salts, and you only have a little salt left with the gold just wash the gold (Search for the thread "getting my gold pure and shinning" use Harold as the author in your search).

After most of the salts were gone, and washing the gold,I would dissolve it back into solution for a proper (or second refining), studying the process well before beginning, and using the sulfamic Lou told you to invest in, if necessary...

Let solutions with gold powders in them settle overnight, and the solution to clear as much as possible before decanting, some salts take time to settle like fluffy silver chlorides and letting the dilute solution set in the cold of the night, will usually leave you with a little more of the salt in the morning


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## Goldman94 (Apr 11, 2020)

butcher said:


> Don't melt any down at this point you could put your gold up in smoke and make it harder to get back.
> 
> It is doubtful the gold dissolved when you added water, but I would do a stannous test of the solution to confirm (I would also check pH and make sure it was at least somewhat acidic before doing a stannous test).
> 
> ...



I've been boiling what I think is my good batch, the one that was yellow and had the majority of gold in it, with just distilled water, since HCL wasn't doing anything at all. The moment I put water in it, half of the salt dissapeared and now I'm on my 2nd boiling and it's starting to form Crystals at the top. I just decanted that solution into another beaker and put more water in to try and rid the sludge of any salts. 

Obviously I'm going to wait awhile until I think most of it is gone and then do a batch of AR and throw it in there and hope I strike gold.

As for my brown solution, I think I'm going to have to continue boiling it down and adding water to it to try and achieve the same thing as this one.

I'm saving all of my decanting solutions just incase anything was left behind, because I'm sure there was


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## butcher (Apr 11, 2020)

I do not understand why your working with two batches?
It is hard for me to follow all of what is going on, I thought you were working with one mess, not two different batches.

Well as long as you understand what your doing.

After collecting all of your washes and solutions (even if they test negative for gold) you will not lose your gold if you follow the instructions to treat your waste for disposal properly. found in the safety section...

Any gold will cement out with copper. You will recover it in this step.
Copper and many of the other toxic base metals are cemented out with an iron.
Many more of the toxic metals are removed by raising the pH to around pH10.
And more metals removed when we bring the salt solution back to neutral around pH 7...


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## Goldman94 (Apr 11, 2020)

butcher said:


> I do not understand why your working with two batches?
> It is hard for me to follow all of what is going on, I thought you were working with one mess, not two different batches.
> 
> Well as long as you understand what your doing.
> ...



So when I was processing everything the other day, before this all happened. I split the AR solutions into 2 batches. One ended up being a golden yellow color and the other ended up being a dark brown color. I did the exact same stuff with both so I was confused as to why they were different colors


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## butcher (Apr 11, 2020)

you may have done the exact same thing, but apparently the chemical reactions formed slightly different.

They could hold different salts of metals, possibly some in different oxidation states, could have previously held different gases, and have made different reactions, possibly the salts may be in different pH ranges...
At this point, colors do not mean much.


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## Goldman94 (Apr 11, 2020)

butcher said:


> you may have done the exact same thing, but apparently the chemical reactions formed slightly different.
> 
> They could hold different salts of metals, possibly some in different oxidation states, could have previously held different gases, and have made different reactions, possibly the salts may be in different pH ranges...
> At this point, colors do not mean much.



It's weird though, since it seems like a good majority of the gold is in the 'good' beaker and it doesnt seem like much is in the other one. There's a little in there but definitely not as much as the yellow one. There's a nice layer of solid gold and, what I hope to be, gold powder at the bottom of this one.

Tomrrow I will try to process it with AR and proceed from that step, adding in nitric little by little this time. 

I believe I have gotten most of the salts out of the solution by adding the water and evaporating them, but if theres still some traces left, how will that affect the AR solution?


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## butcher (Apr 11, 2020)

I would keep everything in one batch and process it together if you have two batch's you have two sources to lose a little bit gold in each batch, the more small batches, with the small losses in each, which adds up over time.

It is better to work with larger batches and keep all of the chemical reactions in one pot as much as possible keeping your eggs in one nest as much as possible and not spread all over the lab...

I put my gold in a corning dish on a hot plate and rarely take it out during recovery and refining, It will see some glassware and filters before being melted, but the gold is pretty much done in the same pot throughout the processes, in one batch keeping the gold in one nest as much as possible.

Traces, or a small amount that will not dissolve after you finish with the recommended process of washing your gold to get it pure and shiny, I would not worry about it, you will clean up the gold more after the second refining.

You may also consider not using aqua regia the next go-around, the gold will be fine enough for HCl and bleach to easily put it into solution after you do a proper washing procedure.


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## Goldman94 (Apr 12, 2020)

So far so good...I did end up splitting the batch, only reason was because I just wanted to make sure that this was going to work. I am currently working on the yellow solution and in will be evaporating everything to thereeee other one and adding in some water a few times to dissolve all the salts and proceed like normal. 

This time I added in about 30ml of HCL then I added in about .5 ml of nitric at a time until all the solids are dissolved. I have just a few specks to go. I will be letting the solution evaporate a little, just to make sure all the nitric is gone. Then I'll go on precipitating the gold and giving it a few washes (hopefully I'll have enough time before it rains)

Till then I'll keep ya guys posted!

Thank you again so much to everyone that has helped me out, I appreciate it more than you know! 

Ps...my ph strips are coming in the mail today, through Amazon, hopefully they still deliver today. Oh also Happy Easter everyone!


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## denim (Apr 12, 2020)

That's the color you want for the quantity of gold you are looking for in that quantity of liquid. The clarity although looks a bit cloudy. Do you have a decent vacuum filter setup? Mine consists of an Erlenmeyer type flask/beaker with a hose connection on the side close to the top. You hook up a handheld brake line bleeding style pump to create a vacuum inside the beaker making filtration go much quicker. I would definitely filter your liquid before dropping with smb etc. You are well on your way to getting some gold.


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## anachronism (Apr 12, 2020)

That looks a lot better. 

Now park the solution and wait until you've got some Sulphamic acid. Letting it evaporate a bit won't get rid of all the Nitric. 8)


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## Goldman94 (Apr 12, 2020)

denim said:


> That's the color you want for the quantity of gold you are looking for in that quantity of liquid. The clarity although looks a bit cloudy. Do you have a decent vacuum filter setup? Mine consists of an Erlenmeyer type flask/beaker with a hose connection on the side close to the top. You hook up a handheld brake line bleeding style pump to create a vacuum inside the beaker making filtration go much quicker. I would definitely filter your liquid before dropping with smb etc. You are well on your way to getting some gold.



You are right, it is very cloudy and unfortunately I do not  
Right now I am filtering it using a coffee filter inside a funnel. I will, however, be getting a vacuum filter very soon.


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## Goldman94 (Apr 12, 2020)

Would this be something like what you are talking about?


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## Goldman94 (Apr 12, 2020)

When I go about rinsing the filter paper off, is there a quantity of water that will be too much as to where I wont be able to drop the gold?


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## jimdoc (Apr 12, 2020)

Goldman94 said:


> Would this be something like what you are talking about?



That will not hold up with acids.


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## Shark (Apr 12, 2020)

If you have silver in the mix, you can add ice to chill it or add three times the volume of water. (Add 300 ml of water for every 100ml of solution) This will drop any silver as a chloride. Add sulfamic acid to stop the nitric, this should also drop any lead as it will convert to sulfuric acid. Then filter. 

Also if you have a piece on hand, use a wad of fiberglass insulation to plug the hole in a regular funnel. Once you get the hang of how tight to pack it, it works great. It is slower than vacuum filtering most of the time, but does a good job. It also takes less water to rinse out. If needed run the solution through the same plug several times, before rinsing the plug, this also saves on adding additional water. You want it absolutely clear of any cloudiness or sediment.


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## Goldman94 (Apr 12, 2020)

Shark said:


> If you have silver in the mix, you can add ice to chill it or add three times the volume of water. (Add 300 ml of water for every 100ml of solution) This will drop any silver as a chloride. Add sulfamic acid to stop the nitric, this should also drop any lead as it will convert to sulfuric acid. Then filter.
> 
> Also if you have a piece on hand, use a wad of fiberglass insulation to plug the hole in a regular funnel. Once you get the hang of how tight to pack it, it works great. It is slower than vacuum filtering most of the time, but does a good job. It also takes less water to rinse out. If needed run the solution through the same plug several times, before rinsing the plug, this also saves on adding additional water. You want it absolutely clear of any cloudiness or sediment.



Ohh not a bad idea on that fiberglass. I have some ceramic fiber insulation that I use for my crucibles, would that work?


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## denim (Apr 12, 2020)

This is the setup I use. Shown here are the setup, a couple picts of pumps (one in a box the other out of the box), funnel with a charmin plug (four squares of toilet paper wadded up and stuffed very tightly into funnel neck). This has worked very well for me at the small scale refining I do. I ordered all these things separately including the rubber stopper with a hole for the funnel.

And yes, this is just to display this setup. I do all my filtering outside.


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## Goldman94 (Apr 12, 2020)

denim said:


> This is the setup I use. Shown here are the setup, a couple picts of pumps (one in a box the other out of the box), funnel with a charmin plug (four squares of toilet paper wadded up and stuffed very tightly into funnel neck). This has worked very well for me at the small scale refining I do. I ordered all these things separately including the rubber stopper with a hole for the funnel.
> 
> And yes, this is just to display this setup. I do all my filtering outside.
> 
> ...



You're awesome. Thank you very much!


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## Goldman94 (Apr 12, 2020)

GUYS LOOK WHAT HAPPENED!! THERES EVEN THE LITTLE PIPE THING TOO!!  

There should only be able 3 more grams missing in the other solution, which may be quite possible


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## Goldman94 (Apr 12, 2020)

Also, when I added SMB to the AR, it didnt fizz at all, I got really scared for a second, but after about 5 minutes everything dropped quite quickly. I was surprised


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## butcher (Apr 12, 2020)

Goldman94.,
Ahh I was expecting to discuss salts and now all you have is that gold  :G 
Good job my frien  d, although you may be moving a little fast, jumping in before you gain a full understanding can lead to problems :twisted: , I know you are anxious to see the gold  , slowing down and gaining a little patience will help you to become a better refine :lol: r, be sure to properly treat your waste. 

I thought I would [play with the emoji faces, boy can't I make a messy post with them


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## Goldman94 (Apr 12, 2020)

butcher said:


> Goldman94.,
> Ahh I was expecting to discuss salts and now all you have is that gold  :G
> Good job my frien  d, although you may be moving a little fast, jumping in before you gain a full understanding can lead to problems :twisted: , I know you are anxious to see the gold  , slowing down and gaining a little patience will help you to become a better refine :lol: r, be sure to properly treat your waste.
> 
> I thought I would [play with the emoji faces, boy can't I make a messy post with them



Thank you so much Butcher for all the help and knowledge you've brought to this thread and forum. 

I've been researching the processes for quite some time now and finally want to put to the test of what I've learned. Like I said earlier, my very first batch came out wonderfully with 0 problems whatsoever. It was this 2nd batch and the addition of baking soda that caused all this. I dont think I'll ever keep baking soda in my house ever again, that's the devil lol. 

I am going to keep practicing on what is the right about of nitric to use in AR and I will add it, probably .5-1 ml at a time. I will also continue reading and researching everything I can out there to make my life, and your guys' life as easy as possible.

Again thank you so much for everyones help, I couldnt have done it without you guys.

Also, I still have that 2nd batch brewing to try and rid the salts from it too. I will proceed with that in the same manner I did with this batch. Although it will take some time since theres probably close to 800ml to go thru.


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## butcher (Apr 12, 2020)

Goldman94,
I have to disagree with you somewhat, I may have contributed a tiny bit to the discussion as long as I have not made it more confusing with a bunch of emoji faces :twisted: and funny looking equations 

Au + 4HCl + 3HNO3 + Cu + Ag + NaHCO3 =  mess + :x Goldman94 +  + No :G + :| salts


It is you that has helped improve the knowledge base of the forum.
Many members can learn something from this thread with your contributions and follow up of working through this problem.


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## Goldman94 (Apr 12, 2020)

butcher said:


> Goldman94,
> I have to disagree with you somewhat, I may have contributed a tiny bit to the discussion as long as I have not made it more confusing with a bunch of emoji faces :twisted: and funny looking equations
> 
> Au + 4HCl + 3HNO3 + Cu + Ag + NaHCO3 =  mess + :x Goldman94 +  + No :G + :| salts
> ...



Thank you butcher, that equation is 100% correct :lol: 

Ps...I also got my ph strips today


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## Goldman94 (Apr 12, 2020)

And this solution is about a 0 on the ph scale lol


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## butcher (Apr 12, 2020)

Luckily, as you have shown with this thread that the equation is reversible.


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## Shark (Apr 12, 2020)

You got some of your "stupid" gold. :lol: :lol: 

Bet you don't think it is so stupid now!


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## Goldman94 (Apr 12, 2020)

Shark said:


> You got some of your "stupid" gold. :lol: :lol:
> 
> Bet you don't think it is so stupid now!



It's some beautiful, highly intelligent gold lmao :lol:


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## Goldman94 (Apr 14, 2020)

Hey guys! I just posted the results of my fiasco in the gallery section. Check it out! 

https://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=28862&p=304419#p304419


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