Palladium cement out with copper

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Rotz

Well-known member
Joined
Sep 2, 2020
Messages
57
Hello Fellas,

I have read a couple of topic but I can't find result like that.
I have nitric treatment stock pot. It is full of saturated with copper.
I read cement tips to make true the process.
Then I try belows,
A- PH=0 saturated with copper. There is black powder. Solution dark green.
WhatsApp Image 2021-01-15 at 11.38.06.jpeg
B- PH=2 with tap water. saturated copper. There is a little bit black powder. Solution dark green. yellowish brown dust.
WhatsApp Image 2021-01-15 at 11.38.06 (1).jpeg
C-PH= 2 with urea. saturated copper. Ther is a little bit black powder. Solution dark green. yellowish brown dust.
WhatsApp Image 2021-01-18 at 14.46.40.jpeg
Dried dust remain. Just I have this photo sorry. I melt yesterday a little bit.
WhatsApp Image 2021-01-18 at 14.52.13.jpeg
I suspected that this yellowish-brown dust would be copper then I filtered then melted. Color is like gray metal color. I guess it is a little bit shiny from silver. What is your comment, what that it is?
I have no DMG. It is very expensive here.
 
Before copper cementation I took AgCl with HCl and NaCl so it may include HCl or NaCl.
I don't know Tungsten but it could be.
I also check with stannous chloride. They are showed brown color.
Main nitric solution used when different batch IC chips treatment.
 
If you can buy Ammonium chloride and sodium chlorate (NaClO3); You can precipitate palladium.

Have you tested with stannous chloride?
 
Hey
Stannous chloride has showed brown. I dont think these precipitators dont work in with excess nitric. Whole solution remained from nitric treatment.
 
Rotz said:
Hey
Stannous chloride has showed brown. I dont think these precipitators dont work in with excess nitric. Whole solution remained from nitric treatment.

To test for stannous chloride, nitric must be removed.
otherwise
For copper, it is brown
For iron, black
 
Rotz said:
This was helpful. I learnt my mistake.

Palladium, platinum

1 ml Solution
2 ml Distilled water
1 ml stannous chloride

Palladium : Green or blue
Platinum : yellow ~ orange
 
yasin1987 said:
Rotz said:
Hey
Stannous chloride has showed brown. I dont think these precipitators dont work in with excess nitric. Whole solution remained from nitric treatment.

To test for stannous chloride, nitric must be removed.
otherwise
For copper, it is brown
For iron, black
Dear Yasin

Saturated HCl with copper if include palladium, it shows the same brown color with stannous chloride?


Sent from my iPhone using Tapatalk
 
I suspected that brown powder could be FeCl3, then I try with magnet the melted metal. Yeah it is iron or nickel. Decreasing the PH bring out Iron or nickel as brown-yellow residue. I don't increase PH from now on.

I guess they are not metalic iron. Because solution has saturated with copper. I don't properly know but it is disappointment.

Thank you
 
Rotz said:
I suspected that brown powder could be FeCl3, then I try with magnet the melted metal. Yeah it is iron or nickel. Decreasing the PH bring out Iron or nickel as brown-yellow residue. I don't increase PH from now on.

I guess they are not metalic iron. Because solution has saturated with copper. I don't properly know but it is disappointment.

Thank you

You can use cyanide to accurately test gold.
In acid, you must eliminate nitric and then test with tin chloride.
As far as I know; Copper does not react with nickel.
Of course, it is better to research this.
 
Very interesting discussion.

I am dealing with exact same scenario right now.

Just reading this I know what my case is:
- excess nitric (both Nitric and AR treatments)
- saturated with copper
- Brown and Black Stannous

awesome!!! I learned how to go now

You guys rock
 
yasin1987 said:
Rotz said:
I suspected that brown powder could be FeCl3, then I try with magnet the melted metal. Yeah it is iron or nickel. Decreasing the PH bring out Iron or nickel as brown-yellow residue. I don't increase PH from now on.

I guess they are not metalic iron. Because solution has saturated with copper. I don't properly know but it is disappointment.

Thank you

You can use cyanide to accurately test gold.
In acid, you must eliminate nitric and then test with tin chloride.
As far as I know; Copper does not react with nickel.
Of course, it is better to research this.
Using cayanide but with no acid to live and have more fun
yes copper not react with nickle.
How much its important to stable the ph in stocpot for copper?
 
Surprised none of the jedi's jumped in earlier... no offense gents, but Y'all are (relatively) new members giving each other advice that is left unfiltered or corrected.

Rotz, why did you raise the Ph of your stockpot solution?

You should have siphoned off most of the solution and added an iron bar to that clear solution to cement copper and other base metals out.
That's the second step of waste treatment. Siphoning off again and raising Ph to form hydroxides comes after that.

Cemented gold and pgm's are black. Silver cement is grey. You leave the black powders in the stockpot to accumulate and process when it's enough.

If you raise the Ph, iron starts to drop first as a hydroxide, the yellow color is rust.
https://images.app.goo.gl/cjHMmbz5NWYJPkBn6

This iron goo is now mixed with your cemented gold and possibly traces of pgm's. Which ruins the whole purpose of the stockpot. Which is getting all and only precious metal traces out of your waste. Leaving the more reactive metals in solution. See reactivity series.

Let it settle, siphon off the clear liquid and add a splash of HCL bit by bit. All non- precious metals like iron and their hydroxides will dissolve. You can leave it in the stockpot and add waste solutions until it's time to make room for more waste.

This is all explained in the Basic Knowledge Must Read Waste Treatment thread:
https://goldrefiningforum.com/phpBB3/viewtopic.php?f=47&t=1300

@Ashir, don't raise the Ph. Leave it acidic.

To all new members: before you try anything, explain your plan to us in a new thread and wait for a reply.
Study and learn how to use the search function. Ask here if your'e lost.

Martijn.
 
To add: Waste solutions containing nitric acid can be used to dissolve more base metals or you can distill the nitric back out for reuse. Even the metal nitrates. A bit more advanced chemistry and you need a lab glass distillation set for that. Waste is only waste once you have no more use for it.
Waste solutions from silver digestions and cementing, or AR gold digestions should not contain any free nitric.
Your precipitate would have dissolved again.
 
And: if there is solid copper left in your stockpot after cementing, there is no free nitric.
No need to test a solution known to be full of copper salts with stannous, it will give such a brown spot, no gold traces will show. They will be in you black powder.
 
Dear Martijn,

Really no offence by me, I just ask to learn what is that. Your post very clear and it is easy going with my experience. I evaluate all of comments without who write. I already has tried small samples. My waste still stands in bucket.
About PH increasing; past posts direct me to try increasing PH. But I understood I shoundn't do because my waste including iron. I have some small parts of black powder. Thank you very much. Your comments literally what I hope.
A question. My AP wastes saturated with copper and base metals, shows a little brown with stannous test. Should I add some precipitator. Because There is no black powder in bottom.

Thank you.
 
Martijn said:
And: if there is solid copper left in your stockpot after cementing, there is no free nitric.
No need to test a solution known to be full of copper salts with stannous, it will give such a brown spot, no gold traces will show. They will be in you black powder.

I took further amount black powder from trying as you can see at the first photo. My total waste ten times more from this sample but it is not include more black powder.
 
Great. we're here to teach and prevent messes and health damage.
First, AP waste? You have so much that you have to dispose of it? How did that happen with only a couple of small tries?
Have you read and understood the AP thread?

Second, no, 'saturated' AP will not contain any precious metals, besides gold foils, unless you keep adding an oxidizer like H2O2. Or you have made AP start up with way too much H2O2. Then black powder will show up in AP.
Saturated AP is dark brown copper 1 chloride with a layer of white-green slime on the bottom. There is very little Cu2Cl left.
Any pm's in solution will cement out on the base metals as black powder. A bucket with AP is in fact also acting as a stockot, cementing out any trace values on the base metals like copper.

Again, study dealing with waste.

No need to test a solution for pm traces when it's known to be full of copper. And you (should) test your waste solutions before adding to the stockpot. Then it's safe to say you know all traces are out. You will not see any result that will tell you something worth while. There is too much copper. You won't see a faint purple or yellow stain in black paint.

There is a BIG difference between recovering and refining.

Recovering: separating most base metals from precious metals in scrap or ore. ( AP, coppercell, nitric digestions, etc)
Refining: separating and purifying the (recovered) precious metals into highly pure metal. (Silver cell, Aqua Regia, selective precipitation followed by thorough washing steps, fire assay, etc)

In your case i would siphon off the clear liquid, add the rest to the stockpot and leave it there to accumulate.

Don't make fresh AP every time with H2O2. Makes no sense. Study, ask, wait for reply, then try.

Martijn.
 
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