# Alloy nugget refining process needed



## Stool (Jul 21, 2017)

Hello all,
I've been finding native alloy nuggets that contain gold, silver, iridium, ruthenium, palladium, platinum, copper iron, and zinc. I know it seems like a lot...
Is there a way I can remove the ferrous metals only and precipitate everything else or is this something I'm going to need to send to a refiner?


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## jimdoc (Jul 21, 2017)

I think an assay to prove if those XRF numbers are correct would be a smart first step.


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## anachronism (Jul 21, 2017)

Most of those readings are spurious. 

Put a copper plate behind the items before taking the next readings and show us the results.


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## Stool (Jul 21, 2017)

Don't take the percentages too literally. I've had 3 seperate xray assays done and the differences between them is pretty big. The same metals do show up on all of them though. Realistically I'm expecting 20% precious metal content, 60% iron, 20% other.


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## FrugalRefiner (Jul 21, 2017)

May we see these nuggets, not just the XRF screen?

Dave


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## Stool (Jul 22, 2017)

Best picture I can get. They have a slight copper colored tarnish that comes off fairly easily.


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## anachronism (Jul 22, 2017)

Stool said:


> Don't take the percentages too literally. I've had 3 seperate xray assays done and the differences between them is pretty big. The same metals do show up on all of them though. Realistically I'm expecting 20% precious metal content, 60% iron, 20% other.



I'd ask how do you know that you are expecting these figures? I'd also suggest that you try what I said and see what happens. I use a similar gun to yours so I'm not just guessing. 8)


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## justinhcase (Jul 22, 2017)

Stool said:


> Don't take the percentages too literally. I've had 3 seperate xray assays done and the differences between them is pretty big. The same metals do show up on all of them though. Realistically I'm expecting 20% precious metal content, 60% iron, 20% other.


At only 20% noble metals I would just try a straight base metal leach.
That will show you how much may be value, and would be the first step to liberating it.
But I hate to have to repeat this sites Reson-Detra but, Have your finished reading Ms Hoke Yet?


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## 4metals (Jul 22, 2017)

Weigh a nugget and add 3 times its weight in silver to it and melt it together, make sure it is molten and becomes a well mixed bead before you remove the heat. Then hammer it flat and dissolve in 2 parts distilled water and 1 part nitric acid. Basically a crude fire assay. Hammering it flat just gives you more surface area for the acid to work, and will bust off any slags if you had to use a pinch of borax to melt it. 

After the acid stops working decant off the acid and what remains will be your PM's. Iron and copper and silver will dissolve in the nitric (if the nitric is too strong the iron will passivate and not dissolve) Anyway this is a simple test and if when you're done there is nothing in the acid you know a little more about the spurious readings Jon referred to. Depending on their concentration in the original piece, palladium and platinum may dissolve as well, but the gold will remain and if it is there after the digestion, come back and we can give you options. 

Ideally use enough so you can actually collect and melt what is left over, then you can use your XRF to get an idea of content.


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## Stool (Jul 23, 2017)

The xrf gun isn't mine. Its at a recycling center that accepts palladium and platinum from catalytic converters. Its an hour away and $3 an assay and hard to get based on there hours and my schedules.
I had 3 seperate pieces assayed. The results were similar for gold and silver on all 3. There were huge differences in the pgm's and iron counts. The worst piece was 70% iron and 15% precious.
I would expect some differences on each piece but it seems a bit on the extreme. I have found a place that does fire assays and think I'm going to get everything double checked


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## mausolfe (Aug 5, 2017)

Simple solution.

1. crush

2. setup quartz working tube

3. place powder in quartz boat

4. heat to several hundred degrees

5. pass 5% H2 diluted in Ar to reduce all metals.

6. chlorinate with HCl at same temp

7. only base metals will become chlorides

8. put into water at pH 2 HCl, only base metals will enter solution 

9. centrifuge remaining metals

10. metals will be pgms.

For purification, repeat without hydrogen and use Cl2 gas in a sealed tube, quartz, and the use chromatographic methods to separate group elements.

See ya

EM, PhD


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## g_axelsson (Aug 5, 2017)

mausolfe said:


> Simple solution.
> 
> 1. crush
> 
> ...


If that is a simple solution then I don't want to know what a hard solution looks like.

A post like this only proves two things...

1. You haven't done any professional refining, at the most you have theoretical knowledge.

2. This is not meant to help the original poster, it's just showing off.

Maybe you have a PhD or maybe you don't. We don't care. On this site experience is all and it is proved by posting useful answers or insightful questions.

By the way, I suspect that your simple solution have three major flaws.
1. It isn't easy to crush an alloy like that into a powder.
2. Silver chlorides will not dissolve in pH 2 HCl and it stays with the precious metals.
3. With an alloy of more than 50% precious metals the alloy will not separate into different metal grains, it will remain an alloy. Centrifuging the remaining precious metal powder is just extracting alloy from any liquid and that is not refining.

Göran


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## Topher_osAUrus (Aug 6, 2017)

g_axelsson said:


> If that is a simple solution then I don't want to know what a hard solution looks like..
> Göran



Isnt there more problems than that Göran?

Like pass H2 dilute in Ar to reduce metals?
-arent they already reduced? They are nuggets...
Or did he mean dilute in air? 
Either way, the metal nuggets are metalic nuggets, not metal salt chunks.

Chlorinate with HCl, isn't that generally done with gaseous chlorine, or another method, like the HCl +bleach method, which liberates chlorine from the HCl?
Or would the "heat to a few hundred degrees" (centigrade, or Fahrenheit, dear doctor?) Actually make the HCl do some magic?

As you mentioned, its already way off base, and impractical to say the least...but, I was just curious if there was something Ive been missing..  . :roll:


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## 4metals (Aug 6, 2017)

> 5. pass 5% H2 diluted in Ar to reduce all metals



Hydrogen gas in Argon. This isn't an everyday backyard technique.


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## g_axelsson (Aug 6, 2017)

There are a lot of problems I guess. I didn't have time to dissect the post any more and never felt a need to point out more problem. That's why I said "major flaws".

Yeah, most of the metals are already in metallic (reduced) state, but iron might be oxidized during "crushing" and also present as inclusions in a nugget. Hydrogen is an effective reducer at high temperature so in a quartz tube furnace it can be used to turn oxides into metals.
The next step would be to turn metals into chlorides with HCl as a gas. "At same temperature", but the temperature isn't specified. A lot of chlorides are volatile, including gold and silver chloride. Maybe HCl at high temperature (unspecified) only reacts with base metals, I don't know.

Dilute in Ar means dilute in argon, an inert gas so there is no oxygen present.

The "simple" procedure requires
- Temperature controlled tube furnace with a quartz tube
- A source of hydrogen gas
- Argon gas
- HCl gas (yes, you can get it in pure gas form)
- A centrifuge
And at this stage we haven't even refined the precious metals and for example any quartz in the nugget will still be there. Then he gives a very sketchy method for refining and separating the metals.
- Chlorine gas
- Use "chromatographic methods" to separate the precious metals, whatever that means

This "simple method" is as close to technobabble as you can get and not the least helpful.
https://en.wikipedia.org/wiki/Technobabble

Göran


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## Platdigger (Aug 7, 2017)

Those are some strange nuggets for sure. What Country were they found in?


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## anachronism (Aug 7, 2017)

Platdigger said:


> Those are some strange nuggets for sure. What Country were they found in?



If they are nuggets then I would suggest Narnia.


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## Platdigger (Aug 7, 2017)

Or Tim Buck Three maybe.


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## rickbb (Aug 9, 2017)

Odd how some of them have a flat bottom. Looks more like poured shot or flake.


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## mausolfe (Jul 17, 2019)

I’m pretty sure it works. For those of you saying it doesn’t. I spent the later portion of a year validating what I told you (process wise) from some dirt off of a volcano.

Results seem appropriate to me.


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## mausolfe (Jul 17, 2019)

Key take always:

1. Base metal removal is key - this can be done in solution or through the gas phase as was previously suggested. Fe2O3 converts quickly at 300C to FeCl3 and can subsequently be used as a chlorine source via decomposition under Ar at or above 800C.

2. Encapsulation is a problem - surface area improves reaction and lowers resonance periods.

3. Some oxides can exist he see hitting them with hydrogen preserves the pseudo-noble metal phases such as Mo. The pgms will remain metals in all conditions of heating via thermal decomposition.

4. Bring the metals to temperature (I like induction)

5. Process back over HCl and collect Au

If done right, you’ll yield what I showed in the photo above.

Good luck! 

PS - haters who talked bad about me when I posted the original process I was working up just have no clue.


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## anachronism (Jul 17, 2019)

mausolfe said:


> PS - haters who talked bad about me when I posted the original process I was working up just have no clue.



Don't be such a snowflake. People disagreeing with you isn't hate. It's disagreement. :lol: :lol: :lol: 

Jon


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## mausolfe (Jul 17, 2019)

Under a microscope you’ll see that these particles are exceptionally small.

I have seen under an SEM that they start as nano-particles but appear to nucleate to micron size following processing and exposure to temperature.

I have learned that if I start with a million grams and the methodology has a separation factor of x100, the process requires three passes to yield metals of similar enrichment 

Obviously this is something to do for fun in the lab when I have time, but I hope my perspective gives you some insight


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## mausolfe (Jul 17, 2019)

anachronism said:


> mausolfe said:
> 
> 
> > PS - haters who talked bad about me when I posted the original process I was working up just have no clue.
> ...



Exactly, I disagree with the language used to convey disagreement with my original idea(s) and for ease of typing simply labeled the individual a hater. 

What matters is that there are viable solutions to recovery metals for recycling or from the environment. 

In my opinion all ideas should be considered and debated - but when that’s not done the same language should be used to describe the accusations. Does the process work or not? Early evidence suggests there is something to be considered


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## mausolfe (Jul 17, 2019)

One more thing - for the original poster

Email privately and I’ll send you over the entire protocol. Thanks for asking such a good question that has kept me thinking for a long time.

Everyone have a great day and I hope everyone gets rich


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## FrugalRefiner (Jul 17, 2019)

mausolfe said:


> One more thing - for the original poster
> 
> Email privately and I’ll send you over the entire protocol.


We would prefer that you share your entire protocol on the open forum. As you said in your previous post, "In my opinion all ideas should be considered and debated". We can't consider and debate your protocol if you don't share it openly. We discourage people from providing refining advice via PM because there is no way for anyone to help critique the process to make sure it is safe and sound.

Dave


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## mausolfe (Jul 17, 2019)

That’s true 

For validation that gold exists I would bombard your sample with neutrons to activate Au-198 firstly.

There is a strong gamma spectroscopy line at 411 keV that is easily detectable. Radiochemical techniques allow for its identification and validation because Au-197 has a huge capture cross section. If abundant in your sample, this will be observed.

The technique is non destructive like SEM but creates nuclear transmutation products that must be allowed to decay. I feel techniques like ICP-MS/AES and XRF are prone to interference in sample concentrations though valuable tools that are available readily.

Once you have confirmation that the material exists, I feel that correlation to other techniques can be validated; does microscopy correlate to mass spectrometry and/xrf or NAA or fire assay . 

Removal of iron for instance. - a brittle sample - created by treatment with hydrogen - usually makes these phases susceptible to hydrogen uptake, powderization, and easily crushes. If already in a metallic state like a button, hydrogen treatment is Beloit be viable but will not reduce iron oxide to a metallic state easily. 

This is why HCl (g) + Fe2O3 —> FeCl3 + H2O is viable when dealing with oxides for pretreatment 

Exposure to HCl releases hydrogen gas and displaces water/oxides during treatment of metals annealed in hydrogen. These metal chlorides should be soluble in dilute HCl. Iron, tin, copper, (titanium if followed up with carbothermic reduction will boil out at about 130-200C in the presence of chlorine and carbon - carbon tet. is a viable carbonating chloride molecule).

Pgms are non-reactive to HCl and so is silica.

Work up using normal techniques following to remelt or keep the powders for subsequent processing such as density fractionation. If rich enough you shouldn’t require much more processing.

This assumes you are starting with possibly a concentrate, mixed alloy or high iron material.

High nickel phases require carbon monoxide to reach refinement from pgms*

That’s my first piece of advice


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## mausolfe (Jul 17, 2019)

Oh yes one more thing

If you have high silica, this will come off with titanium but at like 30C as SiCl4 and will leave pgms as chloro-species.

Cleaning up with hydrogen a second pass will preserve those as metals.

You’ll need a cold finger to trap any silicon or titanium if present and required to be removed in a distillation process


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## g_axelsson (Sep 2, 2019)

mausolfe said:


> PS - haters who talked bad about me when I posted the original process I was working up just have no clue.



:mrgreen: 

I guess 4metals and I just have to retire from the forum... we have finaly been exposed as clueless.

By the way, I have another clue to add to the XRF readings. That XRF-gun falsely reads arsenic as iridium. Proven by testing a mineralogical sample this summer.
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=28009

35% iridium is actually arsenic at some unknown concentrations. It also throws off any other reading as the software tries to compensate for the shielding effect of iridium.

Adding acid or roasting those nuggets might produce arsenic containing gas and smoke. Several of our members have made that mistake and at least two came back and told us about the horrid experience of arsenic poisoning. Irons was one, the other one I don't remember.

Göran


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## FrugalRefiner (Sep 2, 2019)

Irons, Tub Buster: Metal Fume Fever and TODDAZ: Caution new mebers! have all experienced arsenic poisoning.

Sorry you and 4metals have been exposed Göran. :lol: 

Dave


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