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Used Aqua Regia, result is green sludge

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p30504

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Joined: April 9th, 2011, 2:21 am

Post April 9th, 2011, 4:02 am

Used Aqua Regia, result is green sludge

Let me start off by saying I know I'm a sloppy idiot, but I didn't have knowledge of this website before I did what I did. I had about 1 1/2 pds of certain gold fill, and another 2-2 1/2 lbs of probable gold plate, some gold fill and other mystery metals. I got a 5 gallon heavy plastic bucket. Poured in about 6 1/2 LITERS of hydrochloric acid ACS grade and about 1 1/2 LITERS of 70% nitric acid ACS/reagent grade, and then tossed in the 3 1/2-4 lbs of the above materials. I must say the chemical reaction was quite impressive but it quieted down after about an hour. I let it sit for about 24 hours, and because I couldn't find any place that sold pure urea, I found a fertilizer marked 30-10-10, the main ingredient being 34% urea, and and the remainder ingredients were 2 other fertilizers the names of which I don't remember. It was about a 5 pd bag. That turned what had been a beautiful emerald green liquid into a milky liquid that over time separated with the result being about 1/2 milky green sludge and 1/2 being a beautiful emerald green clear fluid. I then tossed in what I had of sodium bisulfate , but nothing happened. I only had maybe a pint of the granular S.B. I've separated the sludge from the emerald green fluid, and here I sit, not knowing if I've screwed things up beyond redemption, or if there is something I can do to still retrieve the gold from one or both of the two solutions I now have. Incidentally, after the acids did their work, it appeared that all the gold had been dissolved, but most of the previously gold fill findings remained (minus any gold layer) and appeared to be lead/tin/zinc or some other base metal. These I simply took and melted down into several large slabs that are heavy and look like lead, tin, zinc or some combination thereof. Other than saying that I should forever stay away from chemistry and dangerous chemicals, does anyone have any idea what I should do now to get the gold out, if possible? PLEASE TAKE PITY AND ANY SERIOUS ADVICE WOULD BE MOST DEARLY APPRECIATED.
STEVE (p30504)
p30504@gmail.com
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glondor

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Post April 9th, 2011, 8:06 am

Re: Used Aqua Regia, result is green sludge

I believe every thing you have is salvageable. The correct course from here is not clear to me but I think you will be advised to either denoxx and try to drop again following a set proceedure or cement out your values and start fresh in a proper procedure. Look for denoxx (1 x or 2in the word denox) and cementing values in the search bar. You should gain some understanding of the situation you are in which will help you to understand how to get out of it. Some one else may chime in with further advise. Do not throw any thing out. Your values are still there, somewhere.
Sodium Metabisulfite
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Harold_V

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Post April 9th, 2011, 3:32 pm

Re: Used Aqua Regia, result is green sludge

p30504 wrote:Let me start off by saying I know I'm a sloppy idiot, but I didn't have knowledge of this website before I did what I did.


Understood. That's a common ailment, but there is a cure. Read Hoke.

and here I sit, not knowing if I've screwed things up beyond redemption, or if there is something I can do to still retrieve the gold from one or both of the two solutions I now have.

As you'll come to understand, it's likely your solutions have no values included. You would ascertain that they do, or do not, by testing with stannous chloride. That's in Hoke, too.

Incidentally, after the acids did their work, it appeared that all the gold had been dissolved, but most of the previously gold fill findings remained (minus any gold layer) and appeared to be lead/tin/zinc or some other base metal.


It is for that reason you likely have no values in solution. A great deal will depend on how soon you separated the solutions from the solids---but if my thoughts are correct, the remaining solids cemented the values, so the gold is now mixed in the resulting sludge.

These I simply took and melted down into several large slabs that are heavy and look like lead, tin, zinc or some combination thereof. Other than saying that I should forever stay away from chemistry and dangerous chemicals, does anyone have any idea what I should do now to get the gold out, if possible? PLEASE TAKE PITY AND ANY SERIOUS ADVICE WOULD BE MOST DEARLY APPRECIATED.

It's a shame you melted the sludge. In order to recover the values, you must repeat the acid treatment. I would suggest you melt the material, then pour it to deep water in a metallic vessel (to prevent the hot material from burning through the bottom, assuming your choice might be plastic). Recover the resulting "corn flakes", which would then be digested in dilute nitric acid.

You have to come to terms with the idea that this material may be a bitch to process. If there is lead and/or tin included, you will have problems. Filtration may be difficult, or impossible. If there is silver present (there most likely is) it will be in solution, which can be recovered with copper, or converted to silver chloride with salt of HCl.

I strongly advise you to read Hoke before you attempt any future processing. Get a firm understanding of what must be done, and why. If you fail to do that, you will have questions at every turn. Most of us can overlook your initial stupidity, for none of us are born with the knowledge to refine, but if you resist the advice tendered and venture forth, not understanding what you're doing, or how it should be done, you will wear out your welcome on this forum very quickly.

Harold
You are what you write.
Wise people talk because they have something to say. Fools talk because they have to say something.
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p30504

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Post April 9th, 2011, 11:59 pm

Re: Used Aqua Regia, result is green sludge

Thank you both for your Replies. I found the website where I can read Hoke's book online for free, and will do exactly that before I do another thing.

Incidently, excuse my poor communication. After the material in the A.R. stopped reacting, I had a beautiful emerald green fluid, and at the bottom of the 5 gallon container there were the were the findings absent any coating of Gold. They simply looked like lead findings. Some had just the barest residual amount of the origional layer of gold. I am somewhat curious as to what this base metal had been that it did not dissolve in the A.R.. But anyway, it wasn't till I put the approximately 5lbs of fertilizer that was 34% urea, and the rest other fertilizers that the mixture became a milky green color. I then added the sodium bisulfate with no change in appearance. After letting the entire mixture sit overnight, the milky green solution had settled to the bottom in a concentrated form and the rich clear emerald green fluid laid on top. I then poured the clear green fluid into a separate container, and the concentrated milky green fluid, which was now more like a "sludge" was kept in the 5 gallon container slowly evaporating into a more and more concentrated substance. The base metal findings absent the gold is what I melted down and poured into bottons that were a white silvery metal that I was able to sand and polish into a sivery like metal of what , I do not know. I AM going to read Hoke and hope that I come to a clear directive as to what I do now, but any opinions as to what is what, while I proceed to read the book, would help reassure me that things will be ok, and may help me in which way to go per Hoke, assuming the book offers different options. Thank you both so much for your consideration and time in responding to my question.

Steve (p30504)
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Harold_V

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Post April 10th, 2011, 12:44 am

Re: Used Aqua Regia, result is green sludge

It's entirely possible that the gold cemented and sloughed off, leaving the surface of the remaining base metal reasonably free of gold, although I would expect that you would have cemented copper, too. Do not look for a bright yellow color----that's not how it cements. It may be as dark as a deep purple, or even black. It will have been combined with copper and other elements that will cement on what ever remained, assuming they were not stainless. I'm assuming that the solution tests neutral, however. It's hard to second guess what has transpired, but so long as you don't discard anything, there's no way you'll lose the values. Key to success will be understanding where they are, and why they are where they are. Hoke will help in that regard, because results are relatively predictable, so long as you know exactly what you did.

Good luck. Do keep us posted on your progress.

Harold
You are what you write.
Wise people talk because they have something to say. Fools talk because they have to say something.
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qst42know

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Post April 10th, 2011, 10:20 am

Re: Used Aqua Regia, result is green sludge

I then tossed in what I had of sodium bisulfate


Sodium bisulfate is not a gold precipitant that I know of, but sodium bisulfite is.

Watch your chemical spelling as a single letter changes everything.
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p30504

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Joined: April 9th, 2011, 2:21 am

Post April 11th, 2011, 9:44 pm

Re: Used Aqua Regia, result is green sludge

The last post re sodium bisulfite vs sodium bisulfate is somewhat encouraging. When I was looking up chemical formulas on the internet before I did this, I noted some said bisulfate and some said bisulfide. More said the latter than the former. I assumed that apparently either one would cause the gold to precipitate. But apparently I was wrong, and as a consequence I have not as yet put in anything to cause the gold to precipitate, although, I'm going to read that book first, because I have no idea if or how well anything would precipitate in the milky green sludge. Thanks everyone.

Steven (p30504)
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qst42know

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Post April 11th, 2011, 10:09 pm

Re: Used Aqua Regia, result is green sludge

There you go again, ate, ite, ide, all different. :roll:

I have made the same mistake.

Hoke explains testing to find your gold. Don't throw away any solids or liquids.

And stay away from mixed blends of lawn food it can only complicate maters.
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dtectr

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Post April 11th, 2011, 10:25 pm

Re: Used Aqua Regia, result is green sludge

Did you add ALL 5 lbs of the fertilizer? :shock: if so, I really have no response to that, only that I wouldn't let you put salt in the beans :lol:
Sodium bisulfate is a dry, granular acid. It is what Sparex-2, the jewelry pickle is made of. Think "dilute sulfuric" (look up lazersteve's Dry Nitric recipe for an example of its proper use.

And I know you didn't mean it that way, but acknowledging that you did something stupid (we all do) then trying to justify it to Yoda (Sorry, harold - couldn't resist 8) ) doesn't sound like a good fresh start. To paraphrase my Dad, one of the wisest men I've ever known - You can't accomplish something good by doing something bad.

You didn't lose Fort Knox, thankfully. Maybe put it in a sealed bucket somewhere with a printout of this thread taped to it. When you've learned what you need to, go back & read it, call yourself some derogatory names, then kick that sludge's a**.
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p30504

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Joined: April 9th, 2011, 2:21 am

Post April 11th, 2011, 11:57 pm

Re: Used Aqua Regia, result is green sludge

I apologize, I really wasn't trying to excuse my ignorance. And by the way I do cook my the same way. My fatal personality flaw is impatience. I want to see the results NOW, and if I don't have everything I need and ready to go, then I have to fight the urge to fill in with whatever sounds like it might do the trick. Now that I've confessed to the mentality of a 12 yr old, I will ad that after I put everything in the A.R., I wasn't going to risk the whole batch with my "shotgun" approach. I did set aside 2/3 - 1/2 of the fluid and left that untouched. So, I have a chance to do right with respect to some mixture. As to the milky green sludge, as I said the milky part settled, leaving beautiful emerald green clear fluid on top. I drained that off and bottled it. As for the sludge, the liquid is quickly evaporating and it will be solid in no time. After read THE BOOK. hopefully I can find the proper ingredients and end up with a pleasing result. Anyway, you people are great and I am glad I found this website. Thanks.

Steven (p30504)
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Flytripper

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Joined: February 10th, 2013, 3:31 am

Post February 24th, 2013, 9:35 am

Re: Used Aqua Regia, result is green sludge

mine is not sludge but green in the end and nothing on bottom, i used all the correct chemicals and amounts, im gonna add more precipitant...BUT question...when using subzero, should i mix it with distilled water and sulfuric acid? the instructions said not to,, kinda
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butcher

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Post February 24th, 2013, 10:52 pm

Re: Used Aqua Regia, result is green sludge

Flytripper,
just from what you wrote here I think you are on the wrong track.
It sounds like you paid good money, for some fertilizer and bad advice.


I say put put a bar of copper metal in the solution, download Hokes book, and study the forum, forget about trying to get gold at this point (but keep collecting scrap), spend some time getting acquainted and understanding of how it supposed to be done.
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Flytripper

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Post February 25th, 2013, 5:28 pm

Re: Used Aqua Regia, result is green sludge

you said im on the wrong track, ok heres how i did it, i collected ALOT pc parts all trimmed, 3 ounces of raw . I used subzero instead of nitric acid , but the subzero is pellets, and it says to make nitric acid with subzero, u use sulfuric acid and boil with muric acid and distilled water, the gold dissolved fine!!!
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Geo

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Post February 25th, 2013, 5:48 pm

Re: Used Aqua Regia, result is green sludge

Flytripper, search for "poor man's AR". "subzero" from what i understand (because ive never bought any) is just sodium nitrate. you can skip the sulfuric acid as its not needed for the reaction. hcl and sodium nitrate together when heated in the presence of metal will create AR, and a very good AR at that. this is the process your trying to use. you should study this process and understand it as well as you possibly can before you try it again. its in your best interest as far as you health and well being if you do some reading before you proceed. AR is one of the simplest and the hardest processes to master. it took me a year on the forum before i even tried it. ive totally messed up many batches trying to figure out exactly what was happening in the reaction. thank god there was the forum to guide me when i couldnt figure out what i did wrong.

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