Ok let just say mistakes were made

timsiggins

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OK let me explain, I made AR the right method, HCL 1st the added nitric little by little until everything is dissolved and I keep it at 80c. Also I had a couple of filters in with the gold. It was getting late so I turn off the heat and let the solution cool overnight and went back to it after work. I looked at the solution and it was a dark brown with the filters on the bottom disintegrated, I mix the solution and realized there was gold flakes still undissolved, the solution was dark brown and opaque with lots of small gold specks though it. so I did this.

1. I Tried to get rid of the filter material with a metal strainer, but realized that I could not do it cuz it was catching too much of the gold solution
2. Rinsed the strainer with water and clean it so all material is back in the solution
3. I had a lot of solution so I boiled it to concentrated a bit
4. Added fresh HCL 200 ml
5. Added Nitric Little by Little, like 50 ml

At this point some of the gold specs where not gone all the way, so what did I do? I kept adding nitric (embarrassed in how much like 25-30ml) 5ml at a time, and still not all sparkly stuff would not dissolved. then I added more fresh HCL about 200ml and more nitric (another 25-50ml, 5ml at a time). Long story made short I had too much Nitric and still sparkly stuff, so I decide to filter and drop the gold


So I put a tiny amount of smb to drop the gold and it was like a grade school science fair project, ya know the one with the volcano and baking soda with vingar. Thank goodness I was being carful and only put a little smb. Ok, with all that being said I know I made lots of mistakes with this one, but this was not my 1st extraction and purification. So that being said, I know uera is for my garden and should stay the heck away from my gold extraction lab but it was late and I was desperate and I did have it around for my garden, I have never had to use it before because I always have been careful about how much HN03 I used. So I used urea :( and in order to get rid of all NH03 and I had to use alot of it :( :(. Finally the smb didnt fizz so much so I was able to use it to drop my gold. Then I left it over night, when the gold settled. well, I grew a crystal garden. So before I go and mess it up even more I thought I would share it with you guys and see what you think

BTW I will use the as a learning lesson so please dont beat me up too bad. Also there is a lot of gold powder under those crystals
 

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Noggin

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That’s pretty!
I was in the weeds over the weekend after an ugly watch band cap recovery with AR chems not acting like they should. I looked for an eject button and settled on copper. After adding copper too fast (not recommended)
I recovered the sludge (full of gold and tragedy), tested for gold in the solution, then incinerated the sludge and started over. Back on track.
For you, I would heat and dissolve the solids, and slowly concentrate to a syrup. Boiling not recommended. Rehydrate with a little HCL and you may be able to drop.
Be sure to test for gold each step (before heating, after dissolution, after rehydrating).

Good luck Tim. Hoke’s book covers this too, by the way.
 

cejohnsonsr1

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Something worth noting is that SMB will eventually remove all of the excess Nitric because as soon as the gold starts to drop the Nitric will redissolve it. Eventually that process will consume all of the excess Nitric, but it is definitely not the best way to go about it. If your AR gets saturated, add HCL to freshen it up. That will usually allow the remaining Nitric to begin reacting again. If you don't get a reaction after adding HCL, you probably don't have any remaining Nitric if there's still undissolved gold. At that point you're probably better off to pour off the solution and start a new AR to dissolve the remaining gold. The thing to keep in mind is that the gold dissolves into the HCL and the Nitric gets consumed by the reaction, so it's the HCL that becomes saturated to the point that it can't bear any more gold no matter how much Nitric you add.
 

vgecas

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i would test liquid for gold, filter out solids, dissolve solids in hot water and filter again while hot.
 

nickvc

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If you used a metal strainer then that strainer will have gold on it as it will have cemented some of your gold.
 

timsiggins

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So I was able to get the gold out by heating the liquid and the crystals melted. Then I let it settle but keeper it warm, then decanted add water and repeat. Now it time to clean it up,
 

Marcel

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Why people still use Urea?
In this forum it has been said over and over again, that it is of no use for the small refiner and it can even blow up.
There are much smarter ways (which you can find here as well) on how to work with Aqua Regia:
0. Start with HCl and only add HNO3 in small increments until no more brown fumes are visible from reaction
1. Super easy: Add some pure gold to AR and you will never overdose that nitric again. Gold is either in solution or in the button. Nothing is lost.
2. Super-duper easy: Add H2O2 . Fantastic effect = No NOx gases are being emitted because:
2NO + 3H2O2 -> 2 HNO3 + 2H2O

So only H2O=Water will be created instead of NOx gases. Did it myself, works great.

Please folks: Read a bit more on what you are doing before you start! I am getting tired of the same old false stuff you may have caught from Youtube makers (who quick and dirty copied some info snippets from this forum)
 

notehunter494

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Hello Marcel and I like your 3 step method. On the addition of hydrogen peroxide: First, what is the concentration? Second, when is this added? I am still struggling with the reactor vessel, a closed system with a 2000ml erlenmeyer and thistle for adding chemicals, or a semi closed system in a tall 2000ml beaker/watch glass covered (like kadriver videos)? I am working on a scrubber now, by how much may I scale it back if the hydrogen peroxide eliminates most or all NOx gases? Will I be scrubbing just Cl gases? My sole operation is processing clean incinerated jewelers bench tray filings consisting of by weight approx. 95% 18k gold with the 5% balance mostly silver with a little platinum and traces of who knows what. So basically a nitric digestion first then after cleanup and filtering an SMB drop for 99.95 gold. The scrubber I am crafting is based on 4metals concept and Kurtak's designs in the Library category: Building Your Own Equipment; thread: Building a chemical fume hood with a plain steel blower, which has the first two columns of hydrogen peroxide and last a third column of sodium hydroxide solution. Thanks
 

Noggin

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Hello Marcel and I like your 3 step method. On the addition of hydrogen peroxide: First, what is the concentration? Second, when is this added? I am still struggling with the reactor vessel, a closed system with a 2000ml erlenmeyer and thistle for adding chemicals, or a semi closed system in a tall 2000ml beaker/watch glass covered (like kadriver videos)? I am working on a scrubber now, by how much may I scale it back if the hydrogen peroxide eliminates most or all NOx gases? Will I be scrubbing just Cl gases? My sole operation is processing clean incinerated jewelers bench tray filings consisting of by weight approx. 95% 18k gold with the 5% balance mostly silver with a little platinum and traces of who knows what. So basically a nitric digestion first then after cleanup and filtering an SMB drop for 99.95 gold. The scrubber I am crafting is based on 4metals concept and Kurtak's designs in the Library category: Building Your Own Equipment; thread: Building a chemical fume hood with a plain steel blower, which has the first two columns of hydrogen peroxide and last a third column of sodium hydroxide solution. Thanks
I realize you are addressing Marcel but the thread is a little old so I’ll take a shot.
You should be inquarting with silver or copper and using nitric first to concentrate your gold and remove all possible silver.
Then you can use HCL with hydrogen peroxide to dissolve gold in a warm solution (I use about 70c). Get stronger stuff than the 3% drug store peroxide if you can (beauty supply stores is where I get mine).
You only release chlorine till you precipitate.
But unless you move to electrochemistry you’ll still need nitric unless you use sulfuric acid but I don’t recommend that at this time.
 

notehunter494

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Thanks Noggin and yes inquarting is almost always the way to go but I am in the unique situation of having this fine consistent size material, lots of surface area. Reading Harold from the Library he would, if I understood him correctly, always boil filings out in nitric rather than inquart, which is a lot more work. That would successfully remove the sterling silver. I would boil in nitric rinse and filter 3 times. I would be left with clean 18k filings with approx. 2 to 3% platinum filings mixed in. From there I can use the HCL with hydrogen peroxide to dissolve it all and toss in a pure gold button to make sure the nitric is exhausted, then drop with SMB. I will start small, maybe 10 grams and move up. I would be happy to process batches in the 2 to 4 ounce size, not more. Thanks for the hydrogen peroxide tip, yes the concentrated stuff. I think pool supply may have it too. Thanks again.
 

Noggin

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Thanks Noggin and yes inquarting is almost always the way to go but I am in the unique situation of having this fine consistent size material, lots of surface area. Reading Harold from the Library he would, if I understood him correctly, always boil filings out in nitric rather than inquart, which is a lot more work. That would successfully remove the sterling silver. I would boil in nitric rinse and filter 3 times. I would be left with clean 18k filings with approx. 2 to 3% platinum filings mixed in. From there I can use the HCL with hydrogen peroxide to dissolve it all and toss in a pure gold button to make sure the nitric is exhausted, then drop with SMB. I will start small, maybe 10 grams and move up. I would be happy to process batches in the 2 to 4 ounce size, not more. Thanks for the hydrogen peroxide tip, yes the concentrated stuff. I think pool supply may have it too. Thanks again.
I thought about whether it was necessary to inquart the filings. If the fillings are not reduced by nitric boils then the fillings are too large. 18k is 25% contaminants and you stated the filings were still 18k. If you take your raw 18k filings and reduce the dry weight by over 10% in nitric then it seems like maybe the nitric is getting good penetration.
It really sounds like you have enough material to try a couple things. Cheers!
 

dkbinco

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Hello guys I just joined today , I have been following along. I have some sulfide gold ore and everything to recover with HTC and Bleach, I have powdered the ore, I am not sure if it is nesassary to wash or roast the concentrate before??? I don't think so. I have a ph, and ROP meter and I am about ready to start, just checking things. I haven't herd of anyone checking ph or keeping the meter reading 1000 and not below 400ma till chlorinated gold solution is done? I chose this method because its one of the first and cheapest. I am enjoying this talk, but will someone verify my attempt to have a chance of working. NO I didn't get an assey yet, but I want to try it (outside with all the PPE and ventalation) because I know it is gold bearing. You all scared me a little with the other minerals or whatever that might be in the ore harmeing me, but dosn't roasting create toxic fumes of its own. Anyhow I would appriciate any kind of input....Thanks
 

Yggdrasil

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An assay is usually something you have done by a lab.
They have the equipment and expertise to do it properly and understand the results.
When you say you know it is gold bearing..
How do you know without an assay?
 

galenrog

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Mixing acids with ores. Not a good idea. If you are lucky, the process will kill you quickly. Get an assay. Consult with a professional on how to proceed based on assay results.

Time for more coffee.
 

Martijn

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Hello Marcel and I like your 3 step method. On the addition of hydrogen peroxide: First, what is the concentration? Second, when is this added?
Those three 'steps' are actually different options to eliminate free nitric or NO gas from solution. Not steps to follow in that order.
The first two are to prevent/eliminate any free nitric so precipitation of gold can be done.
The last one is to prevent the formation of the brown NOx fumes during an AR digestion by turning the gas back into nitric, which has nothing to do with the 'excess of free nitric' problem, but can be used to produce less fumes and get the most effect out of your nitric.
Martijn.
 

Martijn

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You should be inquarting with silver or copper.
Never inquart with copper if you have silver. It uses three times more nitric to digest.
To get the most out of acids, you could inquart with sterling silver, and by doing so, recovering the silver and the gold in one go.
 

dkbinco

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Mixing acids with ores. Not a good idea. If you are lucky, the process will kill you quickly. Get an assay. Consult with a professional on how to proceed based on assay results.

Time for more coffee.
OK thanks I understand, I am retired, wife and I are RockHounds in co and make and sell crafts with minerals and stones we gather. I don't have a lot of extra cash to do assays. How else would you recover gold that small without chemicals, it won't pan. I will look into it. Thanks
 

dkbinco

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An assay is usually something you have done by a lab.
They have the equipment and expertise to do it properly and understand the results.
When you say you know it is gold bearing..
How do you know without an assay?
Yea I know what an assay is, I don't have a lot of cash for stuff right now, but
An assay is usually something you have done by a lab.
They have the equipment and expertise to do it properly and understand the results.
When you say you know it is gold bearing..
How do you know without an assay?
Yea I know what an assay is, ha! Thanks, I just don't have a lot of extra money right now. This ore is from a mine dump and was not viable for them to process at the time. Do you agree I might kill myself to run it through this process to try. I can do 200 g at a time. Small I know, but I will know how much I can recover after cooking the sludge if its under 2 gpt then bad, but I need to know. Thanks. How is a fire assay done? dont they burn it in a crusibl of somekind I mean what different way can I do even if I find out what is in it I still have to get it out someway. I understand I priced one in nevada $60 or so and shipping, Thank you I hope to be able to stay in touch.
 
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dkbinco

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Yea I know what an assay is, I don't have a lot of cash for stuff right now, but

Yea I know what an assay is, ha! Thanks, I just don't have a lot of extra money right now. This ore is from a mine dump and was not viable for them to process at the time. Do you agree I might kill myself to run it through this process to try. I can do 200 g at a time. Small I know, but I will know how much I can recover after cooking the sludge if its under 2 gpt then bad, but I need to know. Thanks.
 

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galenrog

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The fact that the material came from a mine dump does not mean there are recoverable values. How did you determine there was gold in each of your samples?

Back when the world was young, and arthritis had not yet attacked my fingers, I did a lot of lapidary. The most valuable pieces I shaped and polished was a lovely chunk of orange opalite. The source was a now abandoned cinnabar mine. The orange color was from cinnabar, a primary ore of mercury. Over $100 per gram for the finished pieces. I also made cabochons from various ores of copper, gold, and silver. Mostly from things I personally collected. If you have the time and patience to learn lapidary, and do it well, you have an opportunity.

Time for more coffee.
 

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