Problem with Cu/Ag/Pd/Ni nitrate DMG

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zwai

Active member
Joined
Mar 1, 2016
Messages
29
Hello everybody!


My name is Ain and I am new in this forum.

I have learned to recover platinum and gold but I have problem to precipitate palladium from mixed nitrate. I made DMG solution but after I added it to nitrate mixture the solution went dark brown/green. I understand that there is problem with Ph. I added NaOH and now I have some yellow/green sediment bottom of vessel.

Can someone share information what I doing wrong.



Thanks in advance
 
Yellow sediment is Pd-DMG. You may use Na-acetate as a buffer, pH=4.
Most disturbance comes from Ni - gives deep red
 
Thank you Lino1406 for your help. It seems that it worked well!

Can you tell why this solution still dark? As I saw from youtube it should be blue if Cu is presented.
 
Zwai,

You are new here, so welcome to the forum.

If you notice within a half hour of your posting you had the solution to your problem. Lino is a valuable member of this forum, his short and to the point answers help a lot of members. Then you mentioned You Tube. Ughhhhh..... you found this forum, that is good for you. All of your questions can be answered by reading here and studying on the forum. Do yourself a favor, stay away from You Tube. (with the exception of video's posted by members there and linked from this site) You will fill your head with less misinformation and missed process steps by studying here.
 
zwai said:
Thank you Lino1406 for your help. It seems that it worked well!

Can you tell why this solution still dark? As I saw from youtube it should be blue if Cu is presented.
As 4metals said, YouTube can lead you in bad directions. It's just like anything else you find on the internet: it's only worth paying attention to if you know the source is a good one. But I'll not dwell on that further.

Yes, copper can give a blue color--and other metals can give other colors. Any color in your solution will be a mix from all of those indicators together. Your solution is pretty dark--so it's concentrated, but dark what? Dark blue? Dark green? Or perhaps dark purple (red from Ni + blue from Cu)? Take a small amount of your solution and dilute it until you can see what color it is--or hold the beaker to a light if it's just on the edge of "too dark to tell".
 
Thank for advice. I usually read the forum and have read Hoke's book but Hoke do not say anything about palladium nitrate and DMG. Thing is that video was uploaded by kadriver http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=51&t=19062

I have some results but it seems that salt I got are very different from I have seen.

Can someone give advice as my hands are tied. I have about 200kg old phone server pins to recover and DMG seems to be only option.
 
Some pictures.

1. Solution before adding DMG
2. Solution after DMG
3. Pd salts (it seems that something is wrong with color)
 

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Some pictures.

1. Solution before adding DMG
2. Solution after DMG
3. Pd salts (it seems that something is wrong with color)
 

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Hi

If I have Nickel in solution is it possible seperate Pd and Ni separately with DMG adjusting ph?



Thanks
 
zwai,

I noticed you mention mercury in the title, along with copper and palladium. What other metals, what was the source material?.
Was the original material recovered from, or an ore?
How did you eliminate the mercury and base metals?
Did you just make a mess by dissolving this unknown metal in acid and expect a recovery, and just bypassed the recovery stages, going straight into a refining stage?

I am not sure of the material your working with or its source, that information can be helpful.
It is obvious you have other metals involved, and it does not look like you done any recovery stage, before trying to refine a palladium metal or salt?

What methods did you use to eliminate base metals? Or the palladium from the mercury (safely), copper and other base metal?

Mercury in your material concerns me, because of its dangers if the material is not treated properly.
Mercury is also low on the reactive series, so with some methods it will follow your wanted metal with cementation for example.

The pictures lead me to believe you have a solution saturated with base metals, high in copper and other metals, using DMG, with a solution loaded with base metal is not a good idea, dissolving mercury in acids along with your values is not normally a good idea.

You are working with some dangerous chemistry. Watching some videos on you tube and experimenting, without a good working knowledge, or understanding is not a good idea. There are many things you would need to know, background information, and safety information, that a video will not show you. Your material may be different, and may need different methods to recover the values safely. You will not learn the dangers of improperly dealing with waste, or dangerous of metals or materials not included in the video. There is a lot of background information you would need for success. Information and knowledge you will only get from study...

I may be able to watch a video of how someone trouble shoots, and repairs a Television set.
That does not mean I can repair My TV, from what I learned in the video. Especially if I had no electronic background, or knowledge of the safety involved.
With no working experience in the electronics or TV repair field, it would be a mistake to tackle the project from just watching a video no matter how good the video was.
The video may be helpful to a TV repairman who has a working knowledge. But If I tried what I seen in the video, on my TV I could be in for a shock. Most likely my TV would be in worse shape than it was before I started tearing into it, with out really knowing what I was doing.

Not knowing where the mercury is, or how you handled it, it would be hard to make suggestions, of what to do next with your solution or remaining powders.

Not knowing what metals or material you dissolved originally, or knowing more of the details of what you have done, it is also hard to say how to recover values from the salts or complex, (mess you have on your hands now) or how to deal with these toxic wastes safely.


Not knowing if you even had palladium, or what metals the original metal was before you dissolved it into nitric acid, it is hard to give a better method of recovery.

I am reluctant to tell you to dry and save the powders, and cement the solution and save those powders, until you study more, because of the unknown mercury content.

Trying what you see in a video before you learn more of recovery and refining, and safety needed, can, and will put you in dangerous situations, and most of the time it will not be successful.

I do not know what you have, from the solution loaded with base metals (and possibly mercury), for all I know you may have just lowered the pH and have a mix of base metal hydroxides along with the possibility of some palladium DMG complex.

After dealing with mercury properly in a recovery stage. Then a recovery stage of removing base metals. Or a recovery of palladium with zinc, or copper cementation. Before going into a refining stage. May have been a better option, before trying to recover palladium with DMG. But again without knowing what you had to begin with it is hard to say.

Read Hokes.

Give more details, maybe the forum members can help you safely deal with this dangerous mess you have on your hands now.
 
butcher said:
zwai,

I noticed you mention mercury in the title, along with copper and palladium. What other metals, what was the source material?.
Was the original material recovered from, or an ore?
How did you eliminate the mercury and base metals?
Did you just make a mess by dissolving this unknown metal in acid and expect a recovery, and just bypassed the recovery stages, going straight into a refining stage?

I am not sure of the material your working with or its source, that information can be helpful.
It is obvious you have other metals involved, and it does not look like you done any recovery stage, before trying to refine a palladium metal or salt?

What methods did you use to eliminate base metals? Or the palladium from the mercury (safely), copper and other base metal?

Mercury in your material concerns me, because of its dangers if the material is not treated properly.
Mercury is also low on the reactive series, so with some methods it will follow your wanted metal with cementation for example.

The pictures lead me to believe you have a solution saturated with base metals, high in copper and other metals, using DMG, with a solution loaded with base metal is not a good idea, dissolving mercury in acids along with your values is not normally a good idea.

You are working with some dangerous chemistry. Watching some videos on you tube and experimenting, without a good working knowledge, or understanding is not a good idea. There are many things you would need to know, background information, and safety information, that a video will not show you. Your material may be different, and may need different methods to recover the values safely. You will not learn the dangers of improperly dealing with waste, or dangerous of metals or materials not included in the video. There is a lot of background information you would need for success. Information and knowledge you will only get from study...

I may be able to watch a video of how someone trouble shoots, and repairs a Television set.
That does not mean I can repair My TV, from what I learned in the video. Especially if I had no electronic background, or knowledge of the safety involved.
With no working experience in the electronics or TV repair field, it would be a mistake to tackle the project from just watching a video no matter how good the video was.
The video may be helpful to a TV repairman who has a working knowledge. But If I tried what I seen in the video, on my TV I could be in for a shock. Most likely my TV would be in worse shape than it was before I started tearing into it, with out really knowing what I was doing.

Not knowing where the mercury is, or how you handled it, it would be hard to make suggestions, of what to do next with your solution or remaining powders.

Not knowing what metals or material you dissolved originally, or knowing more of the details of what you have done, it is also hard to say how to recover values from the salts or complex, (mess you have on your hands now) or how to deal with these toxic wastes safely.


Not knowing if you even had palladium, or what metals the original metal was before you dissolved it into nitric acid, it is hard to give a better method of recovery.

I am reluctant to tell you to dry and save the powders, and cement the solution and save those powders, until you study more, because of the unknown mercury content.

Trying what you see in a video before you learn more of recovery and refining, and safety needed, can, and will put you in dangerous situations, and most of the time it will not be successful.

I do not know what you have, from the solution loaded with base metals (and possibly mercury), for all I know you may have just lowered the pH and have a mix of base metal hydroxides along with the possibility of some palladium DMG complex.

After dealing with mercury properly in a recovery stage. Then a recovery stage of removing base metals. Or a recovery of palladium with zinc, or copper cementation. Before going into a refining stage. May have been a better option, before trying to recover palladium with DMG. But again without knowing what you had to begin with it is hard to say.

Read Hokes.

Give more details, maybe the forum members can help you safely deal with this dangerous mess you have on your hands now.

Thanks Butcher

At first I must apologize as it is no Hg but Ag (Silver) ... my mistake. I have read Hoke and it was very useful for gold and platinum recovery as well I searching info from this forum. I have tried to find information about palladium recovery from nitrate but there is little information out there.

We got a old 70's land phone server as well NMT server from 1995 (Nokia DX200). All these systems are builded up mainly with palladium. I never recover palladium so I have no experience on with this metal.

I read that best way to eliminate base metals is to use Nitric acid but it dissolves palladium as well. So my option was to use DMG. All this mess on the pictures came from these details (pic1,2). I made a test with ammonia to clean up salt and all salts I got were green ( I think it is nickel (pic3)). Stannus show Pd positive.

I hope you can help me out.


Thanks in advance
 

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Barren Realms 007 said:
Look into using sodium chlorate for your Pd.


Greetings Barren Realms 007

Does NaClO3 separate Pd from nitric? How this process looks like?



Regards
 
zwai said:
Barren Realms 007 said:
Look into using sodium chlorate for your Pd.


Greetings Barren Realms 007

Does NaClO3 separate Pd from nitric? How this process looks like?



Regards

Here are the results from Lazersteves website search and from the forum search that will give you plenty to read up on it.

https://www.google.com/search?hl=en&as_q=sodium+chlorate+&num=1000&ft=i&as_sitesearch=goldrefiningforum.com&as_qdr=all&as_occt=any&gws_rd=ssl

http://goldrefiningforum.com/phpBB3/search.php?keywords=sodium+chlorate&terms=all&author=&sv=0&sc=1&sf=all&sk=t&sd=d&sr=posts&st=0&ch=300&t=0&submit=Search
 
Barren Realms 007 said:
zwai said:
Barren Realms 007 said:
Look into using sodium chlorate for your Pd.


Greetings Barren Realms 007

Does NaClO3 separate Pd from nitric? How this process looks like?



Regards

Here are the results from Lazersteves website search and from the forum search that will give you plenty to read up on it.

https://www.google.com/search?hl=en&as_q=sodium+chlorate+&num=1000&ft=i&as_sitesearch=goldrefiningforum.com&as_qdr=all&as_occt=any&gws_rd=ssl

http://goldrefiningforum.com/phpBB3/search.php?keywords=sodium+chlorate&terms=all&author=&sv=0&sc=1&sf=all&sk=t&sd=d&sr=posts&st=0&ch=300&t=0&submit=Search


Thanks Barren Realms 007!

I found a way to process larger quantities at first I need to remove Ag with HCl and then add copper sheet to solution. Problem is that I made test and add HCl to solution there is no silver chloride separation at all. Solution color changes from blue to green. I know that I had separated AgCl with HCl but this time nothing happens. Can I add directly copper to my mixed solution to remove Pd? Do Ni precipitates with palladium? I understand that Ni is before Cu on periodic table but maybe it reacts as Zinc does.


Thanks advance
 

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If this solution is from just dissolving the parts in nitric and you get no silver chloride form with the addition of HCl there is no silver in the solution.
Did you fully digest the starting material because if you didn't much of your values could have cemented back out of solution, palladium is not keen on been cemented quickly or without agitation so that might explain why you have some palladium.
 
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