Gold will not drop

[sleepyman1]

Sorry for the late reply. The copper stopped dissolving. The solution is as black as used motor oil. I drained off the solution to take a look at the bottom. There was a tiny amount of blackish powder at the bottom. About as much as an aspirin. The ph is at about 4. The stannous test looks hopeless. Should I decrease the solution back down to 1 or 2 ph and keep going? Or call it a loss and move on?

The left sample is before adding the stannous. The stannous was freshly made.

 

[sleepyman1]

To help Kurt out, maybe this thread should be copied in to one without all the sidetracks to stay focussed and keep it manageable.
This is turning into a monster for Kurt.
And way to confusing for sleepyman imo.

I agree!

 

[kurtak]

The copper stopped dissolving.

Ok - we are done with the cementing process on this solution
(stannous test shows no gold)

There was a tiny amount of blackish powder at the bottom. About as much as an aspirin.

That may (or not) be "some" of your gold so hang on to it - we will come back to it later

The solution is as black as used motor oil. I drained off the solution to take a look at the bottom

color doesn't matter - just set it off to the side & let it sit for the next couple weeks - there maybe ultrafine solids (including "maybe" gold) that will take "time" to settle out - so we will come back to it later

Also - back on Feb. 20 on page 5 you posted the following post (that I am quoting here) with two pics of the copper you were using for cementing

Is this what cementing is supposed to look like? This only after about 2 hours of letting the copper sit in the solution with heat.

In those pics - near the top of the copper bar - there is what appears to be gold on that copper (the light brown tan)

what did you do with that copper ?

Now then - we can start looking at the solids left over from the original solutions

It has been quite awhile since we last talked about them - so you will have to give me some time to go back & look at what was posted about them --- likely wont get to that until this weekend

Kurt

 

[sleepyman1]

In those pics - near the top of the copper bar - there is what appears to be gold on that copper (the light brown tan)

what did you do with that copper ?

I used all of it in the solution. That was the first piece I used.

 

[sleepyman1]

My god sorry for being gone for so long. Life gets in the way sometimes.

OK. Kurt I let things settle just like you said. I checked often until nothing settled anymore in the solution.
I dissolved the SMB crystals. Lowered the ph to 2, added copper and almost nothing settled.
I gathered the sediments, washed, dried and threw in the crucible.

FINALLY 22 grams!

The greenish stuff if from my crucible. I need to get a new one and then smelt again.

Thanks to everyone who helped. A HUGE thanks to Kurt!

It will be a long time before I can collect anymore fingers but, I've learned so much that the next time should go much more smoothly.

 

[kurtak]

FINALLY 22 grams!

AWSOME !!!

Glad I was able to help

Most important - we were able to get your gold back from a very difficult mess created (no fault of yours) by the bad, incomplete, & mis-information floating around out there on the internet & YouTube videos that cause these kind of problems in the first place

Your not the first to come here with such a problem & I am sure you won't be the last

But that why we are here

I've learned so much that the next time should go much more smoothly.

In as much as it's good to see you got your gold back - what you learned in going through all of this is where the real value is

Thanks for posting your results !!!

Kurt

 

[swaminair]

That is so absolutely wrong it is in fact false information

Depending on the fingers - (ram fingers - fingers from cards - or a mix) you should get a bare minimum of a gram per pound & more then likely between 1.5 to 2 grams & that is from modern day fingers

Older fingers can even run as high as 3 - 5 grams per pound

If all you got was less then a gram from 10 pounds of fingers - you did something VERY wrong & you lost MOST of your gold



Again - absolutely wrong - from modern day fingers you should get "at least" 1 gram per pound if not 1.5 grams per pound

If all you are getting is 1 - 1.5 grams per 10 pounds you are doing something VERY wrong & loosing MOST of your gold

Concerning the older stuff (fingers) it is not uncommon to see them run as high as 2.5 - 3 grams per pound & I have even seen (though less common) some stuff (fingers) run as high as 5 grams per pound

Same thing with old pins - they can & will run 3 - 5 grams per pound - I have seen old pins plated so heavy that the acid has a hard time getting to the base metal to dissolve the base metal away - in fact the plating can be so thick - that once the base metal is dissolved away - the gold foils will hold their shape & look just like the pins before the base metals are dissolved away

As an "experienced" refiner - running LARGE batches of fingers & pins - for 10 years - as a living --- I will gladly buy ALL of your fingers & pins (provided the pins are fully plated) based on the numbers you are providing

In other words - based on 1 - 1.5 grams per 10 pounds - I will pay (gladly) the high end of 1.5 grams per 10 pounds

Kurt

Thank you mate for the best clarification and information.
Great souls.
regards
swami nair

 

[dasfasf]

Nah, I've just researched the heck out of various possible gold deposits and natural mechanisms of reducing gold in situ. When you actually get out into the field and look at the vast area of rocks and trees... it all becomes overwheming! It's simply a cool this to look for if you find a vein that look promising, especially if there are sulfides. Scrap some material around any oak roots (or black walnut) piercing the rock, especially if there's a lot of organic-looking brown staining from them, it might tell you something useful.

You can use black walnut husks and shells as a source of hydroquinones too. There are some protocols for the extraction. BUYING hydroquinones are expensive, and the high purity of lab-grade isn't necessary for this sort of method.

This autumn when there are lots of black walnuts, I may try the entire protocol from start to finish and see how it works on a modestly dilute gold solution to recover organic-gold complexes as the red-brown goo.

Hi Alondro
can you give me a reference or hydroquinone protocol of walnut or reference?
tanx

 

[Alondro]

Hi Alondro
can you give me a reference or hydroquinone protocol of walnut or reference?
tanx

Having a hard time finding that old article. Most of the references for reducing gold with hydroquinone are newer and regard using quinones to make nanogold suspensions for biological applications.

This new process for cleaning gold out of e-waste uses hydroquinone as the final step in the recovery to reduce the gold, and then the paper describes the recovery of the gold nanoparticles. https://www.sciencedirect.com/science/article/abs/pii/S0957582022008680

The paper has references which describe the hydroquinone process. From the abstract: "Hydroquinone (C6H4(OH)2) has been used as an agent to reduce the oxidation number of metal cations (metal-ion salt solution) to form metal nanoparticles in the presence of metal seeds (Perrault and Chan, 2009). It has also been employed in the reduction reaction (Au+,3+→ Au0) of a gold-salt solution to form gold nanoparticles (AuNPs) (Malel and Mandler, 2008). In the presence of hydroquinone and NaOH, but without metal seeds, AuNPs rapidly form under acidic conditions (Sirajuddin et al., 2010). HAuCl4 solution was firstly mixed with hydroquinone, and then NaOH was added to this mixture to change the pH, resulting in the formation of AuNPs. The addition of NaOH to the mixture has been proved to be able to improve the ability of hydroquinone to reduce the oxidation number of gold ions to form a gold nucleation center, resulting in the formation of 20-nm-diameter AuNPs (Sirajuddin et al., 2010)."

 

[dasfasf]

Having a hard time finding that old article. Most of the references for reducing gold with hydroquinone are newer and regard using quinones to make nanogold suspensions for biological applications.

This new process for cleaning gold out of e-waste uses hydroquinone as the final step in the recovery to reduce the gold, and then the paper describes the recovery of the gold nanoparticles. https://www.sciencedirect.com/science/article/abs/pii/S0957582022008680

The paper has references which describe the hydroquinone process. From the abstract: "Hydroquinone (C6H4(OH)2) has been used as an agent to reduce the oxidation number of metal cations (metal-ion salt solution) to form metal nanoparticles in the presence of metal seeds (Perrault and Chan, 2009). It has also been employed in the reduction reaction (Au+,3+→ Au0) of a gold-salt solution to form gold nanoparticles (AuNPs) (Malel and Mandler, 2008). In the presence of hydroquinone and NaOH, but without metal seeds, AuNPs rapidly form under acidic conditions (Sirajuddin et al., 2010). HAuCl4 solution was firstly mixed with hydroquinone, and then NaOH was added to this mixture to change the pH, resulting in the formation of AuNPs. The addition of NaOH to the mixture has been proved to be able to improve the ability of hydroquinone to reduce the oxidation number of gold ions to form a gold nucleation center, resulting in the formation of 20-nm-diameter AuNPs (Sirajuddin et al., 2010)."

Thank you Alondro, but I meant the walnut protocol

 

[Alondro]

Thank you Alondro, but I meant the walnut protocol

It might be found here! Hydroquinone

I also found this protocol: https://www.researchgate.net/public...ction_of_anthraquinone_from_walnut_green_husk

Anthraquinone can then be converted to hydroxyquinone via various processes, including electrochemistry which is explained in this paper that is so complex it makes my head hurt: Electrochemical Reduction of Quinones in Different Media: A Review

 

[dasfasf]

It might be found here! Hydroquinone

I also found this protocol: https://www.researchgate.net/public...ction_of_anthraquinone_from_walnut_green_husk

Anthraquinone can then be converted to hydroxyquinone via various processes, including electrochemistry which is explained in this paper that is so complex it makes my head hurt: Electrochemical Reduction of Quinones in Different Media: A Review

Very Good Alondro

 

[BGDOCK]

Assuming the only acid you used was HCl, the white sand is probably silver chloride
My recommendations:
1. Make gold test solution using tin solder.
2. Test your liquids for dissolved gold.
3. If no dissolved gold - filter all the solids
4. Take the filtrate, boil in water
5. Filter again
6. Treat filtrate with HCl only. If liquid does not turn blue/green/black. Move on to 7. Otherwise, keeping treating with acid and filtering
7. I hate the bleach method. Do this instead: purchase sodium nitrate and sulfuric acid. Take your filtrate with brown and white solids and add to large beaker. For a 2000mL beaker add: filtrate + some sodium nitrate, then slowly add 500 mL muriatic acid (HCl). Carefully using a dropper add slowly 100mL sulfuric acid (small amounts at a time).
The liquid should turn orange, forming aqua regia. The sulfuric acid helps remove lead. Gently heat, observe to see if all the brown dissolved. If no, try adding a little more sodium nitrate. When all the brown dissolved, heat until no NOX is forming.
Let cool and test with gold test solution. Filter the solution. The liquid passing through the filter should be dissolved gold. Drop and repeat

How many times would you filter and treat w/HCl and what color are you looking for in step 6. ?
Thanks

 

[Yggdrasil]

How many times would you filter and treat w/HCl and what color are you looking for in step 6. ?
Thanks

Hi I see this is your first post, welcome to the foum.
Your question here says you are not ready to start using chemicals yet.
Here is what we like our new members to do first.

We ask our new members to do 3 things.
1. Read C.M. Hokes book on refining jewelers scrap, it gives an easy introduction to the most important chemistry regarding refining.
It is free here on the forum:
https://goldrefiningforum.com/phpBB3/viewtopic.php?f=54&t=197982. Then read the safety section of the forum
3. And then read about "Dealing with waste" in the forum

Regarding your question, this depends a lot on the situation.
What material it is and what has been done to it.
This advice was a bit out of context if I remember correctly.

point 6 was about washing until no more dissolves, which means no color to the liquid.

What do you want to do and why.
Give us a short description and we can give some pointers.

 

[BGDOCK]

1.) check, yes I have bought the book and have read it ( rereading as well)
2.) Will do
3.) I do treat my wastes , I seem I have recovered more copper ( using rebar to cement out Cu)

I had asked for clarification/ more details because I had trouble .

I had performed 2 trail runs one with AP on gold fingers the other with magnetic and non magnetic pins.
I combined the two batches and used the HCl & Bleach method to dissolve the gold ( there was some copper I think in the filter media )

I put the filter media in a HCl and bleach solution it was a yellow green color at first but turned black after heating it Stanous solution showed gold in solution but it was a small amount .
My mistakes:
1.) filtration work needs improving
2.) don’t heat HCl / bleach solution
Since the amount was small I just put in the stock and will cement it out w/ copper .

The picture attach was before added the batch of pins .

 

[BGDOCK]

I have to edit some things
The picture is on the gold fingers batch. To this I added the second batch of pins with the filter media.
I think it was contaminated.
Would it be better to have used Iron Sulfate to drop the gold in this situation?
I not trying to be snarky or rude by any means sir but if you don’t experiment with the chemical and methods how would you learn?

 

[Yggdrasil]

1.) check, yes I have bought the book and have read it ( rereading as well)
2.) Will do
3.) I do treat my wastes , I seem I have recovered more copper ( using rebar to cement out Cu)

I had asked for clarification/ more details because I had trouble .

I had performed 2 trail runs one with AP on gold fingers the other with magnetic and non magnetic pins.
I combined the two batches and used the HCl & Bleach method to dissolve the gold ( there was some copper I think in the filter media )

I put the filter media in a HCl and bleach solution it was a yellow green color at first but turned black after heating it Stanous solution showed gold in solution but it was a small amount .
My mistakes:
1.) filtration work needs improving
2.) don’t heat HCl / bleach solution
Since the amount was small I just put in the stock and will cement it out w/ copper .

The picture attach was before added the batch of pins .

I recommend reading the version I gave you a link to, it has been edited to remove some dangerous practices they had pre 1940s
The reason you get in trouble is usually because you did not do things right and did not recognize the signs of your mistakes.
That is the reason we ask you to study these things.
The HCl/Bleach method needs you to be on the ball all the time.
You need to check the pH often so you do not over add the Bleach and you need to go slow and cold
to maximize the time the Chlorine is available in the liquid.
And if you did not dissolve all metals some of the Gold might have cemented out on the remaining metal.

 

[Yggdrasil]

I have to edit some things
The picture is on the gold fingers batch. To this I added the second batch of pins with the filter media.
I think it was contaminated.
Would it be better to have used Iron Sulfate to drop the gold in this situation?
I not trying to be snarky or rude by any means sir but if you don’t experiment with the chemical and methods how would you learn?

First of all the solution needs to be filtered crystal clear before precipitating anything.
For SMB and maybe Copperas too the solution needs to be sufficiently acidic, something that is not always the case when using the HCl/Bleach method.

Edited forgot always in the text

 

[Yggdrasil]

I have to edit some things
The picture is on the gold fingers batch. To this I added the second batch of pins with the filter media.
I think it was contaminated.
Would it be better to have used Iron Sulfate to drop the gold in this situation?
I not trying to be snarky or rude by any means sir but if you don’t experiment with the chemical and methods how would you learn?

You learn by reading and studying then doing acquaintance testing.
Maybe post your plans here so we can adjust what is needed.
But only after you have studied the safety and waste treatment section.

Where are you performing these tests?
In a lab, shed, garage or other?

 

[BGDOCK]

I recommend reading the version I gave you a link to, it has been edited to remove some dangerous practices they had pre 1940s
The reason you get in trouble is usually because you did not do things right and did not recognize the signs of your mistakes.
That is the reason we ask you to study these things.
The HCl/Bleach method needs you to be on the ball all the time.
You need to check the pH often so you do not over add the Bleach and you need to go slow and cold
to maximize the time the Chlorine is available in the liquid.
And if you did not dissolve all metals some of the Gold might have cemented out on the remaining metal.

Thank you very much
Lessons learned so far
1.)Totally agree w/ you about checking the Ph going slower.
2.) Go cold when using HCl and bleach
3.) being on the ball every second should be a mantra .
4.) bought Nitric Acid yesterday