# Problem with Cu/Ag/Pd/Ni nitrate DMG



## zwai (Apr 11, 2016)

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


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## Lino1406 (Apr 11, 2016)

Yellow sediment is Pd-DMG. You may use Na-acetate as a buffer, pH=4.
Most disturbance comes from Ni - gives deep red


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## zwai (Apr 11, 2016)

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.


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## zwai (Apr 11, 2016)

pic of solution


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## 4metals (Apr 11, 2016)

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.


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## upcyclist (Apr 11, 2016)

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".


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## zwai (Apr 12, 2016)

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.


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## zwai (Apr 12, 2016)

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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## zwai (Apr 12, 2016)

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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## zwai (Apr 12, 2016)

Solution after DMG


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## zwai (Apr 12, 2016)

Hi

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



Thanks


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## butcher (Apr 12, 2016)

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.


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## zwai (Apr 12, 2016)

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?
> ...



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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## zwai (Apr 12, 2016)

Pic2


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## zwai (Apr 12, 2016)

Pic 3 (where Ni salt at the bottom)


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## Barren Realms 007 (Apr 12, 2016)

Look into using sodium chlorate for your Pd.


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## zwai (Apr 12, 2016)

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


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## Barren Realms 007 (Apr 12, 2016)

zwai said:


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



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


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## zwai (Apr 13, 2016)

Barren Realms 007 said:


> zwai said:
> 
> 
> > Barren Realms 007 said:
> ...




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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## nickvc (Apr 13, 2016)

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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## zwai (Apr 13, 2016)

nickvc said:


> 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.




Thank you for reply Nickvc!


I added starting materials slowly to Nitric acid until it reaction was over and some pins were still in solution. I poured off used nitric solution before added additional nitric to pins so I think all Nitric is used. Is it so that if there is free nitric acid in solution HCl do not give out silver chloride? And can you tell me do I need to adjust solution ph before I add copper plate to cement palladium?


Thanks in advance


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## zwai (Apr 13, 2016)

If someone can give me advice for some payment, please let me know!


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## nickvc (Apr 13, 2016)

Just to be totally clear all your starting material was dissolved in the nitric?
If that is correct any silver would now be in solution along with the palladium and other base metals.
If that is the case then when you add HCl the silver will form silver chloride, if that didn't happen you have no silver in solution, there was no silver there to start or the addition of lye precipitated it out in the sludge you mentioned on your first post.
If this material has palladium points not plating it might well pay to clip off as much base metal as you can to start, if there is silver then my suggestion would be to dissolve a small amount of clipped off pins 25 grams say in nitric, filter add either salt or HCl to form silver chloride if there is any silver there, filter to remove the solution and cement the solution with copper to collect the palladium, as I said before PGMs can be difficult to cement so put an air bubbler in the container to keep things moving.
Be aware PGM salts can be very toxic so I prefer to cement collect the powders and melt and sell on.

It might help others to help you if you post pictures of exactly what you are working on, dissolving, I'm fairly sure someone on here has worked with similar materials before.


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## zwai (Apr 13, 2016)

nickvc said:


> Just to be totally clear all your starting material was dissolved in the nitric?
> If that is correct any silver would now be in solution along with the palladium and other base metals.
> If that is the case then when you add HCl the silver will form silver chloride, if that didn't happen you have no silver in solution, there was no silver there to start or the addition of lye precipitated it out in the sludge you mentioned on your first post.
> If this material has palladium points not plating it might well pay to clip off as much base metal as you can to start, if there is silver then my suggestion would be to dissolve a small amount of clipped off pins 25 grams say in nitric, filter add either salt or HCl to form silver chloride if there is any silver there, filter to remove the solution and cement the solution with copper to collect the palladium, as I said before PGMs can be difficult to cement so put an air bubbler in the container to keep things moving.
> ...



Thank you Nickvc

Yes starting material was totally dissolved by Nitric acid. I thought there must be silver as well so a tried to add HCl to solution as well salt and nothing happened. I thought ph is wrong so silver do not come down or I have excess of nitric acid. So if I have tried all options to remove silver and there is no reaction it equals no silver in my solutions? 

I read from forum topic that it is easier to use copper and bubbler so I certainly use this option as DMG salts are not good option for me. 

Yes I add lye after DMG as I read that solution ph needed to be 4 before adding DGM. Even I add small amount lye nothing happened but after large amoun some white layer formed top of solution. I think it is undissolved lye. 

But yes as I see there is no silver so I use better way to cement palladium. Only problem is Ni ... is it cementing with palladium if I add copper plate to solution?


I will make some additional pictures.

Regards
Ain


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## zwai (Apr 13, 2016)

Hi.

I made some pictures of phone servers. They are taken apart. Other pictures are circuit boards from servers. All pins have very little gold layer on them.


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## UncleBenBen (Apr 13, 2016)

zwai said:


> Only problem is Ni ... is it cementing with palladium if I add copper plate to solution?
> Regards
> Ain



No. Copper will not cement Ni from solution since Ni is higher in the reactivity series than copper.


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## nickvc (Apr 13, 2016)

If they are old eastern block telephone equipment they are normally very high yielding for gold and PGMs from what I have seen, the PGMs will be either small dots or dashes on some of the relays, if there are switches check them also, in fact test all places where the use of precious metals could be an advantage even if only a small one.
The newer Nokia material I'm sure others can help with identifying where the best material is to be found, be aware of collectors values on older equipment sometimes it pays better to sell items rather than refine them.

The ph of your nitric solution will make no difference to forming silver chloride and while the Pd will go into solution any Pt alloys will remain as solid pieces, Pt and Rh are not keen to dissolve even in hot Aqua Regia so perhaps once you have dissolved the base metals and Pd filter the solution and recover the Pt from the filter paper.
If you wish to refine your PGMs make sure you know what your doing as I have said before they produce some very toxic salts, also to get high quality you need clean saturated solutions to precipitate the salts from so you Amy have to process them several times.


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## Lou (Apr 13, 2016)

I've done a lot of those little fella's. There should be no silver.

Addressing your present situation--use fresh metallic material (feedstock) to cement out or reduce the mess you have, check to be sure the Pd is removed, filter all that lot of material. You can basically use these metallics over and over to concentrate the Pd before melting and granulating to re-dissolve.

Alternatively, you can adjust the pH of all of your liquors to 8 with lye, getting all metals, inclusive of Pd out of solution (unless, heavens forbid you have ammonium or ammonia in the solution, in which case your only option is cementing). Then, when you trim up the pieces and do the nitric dissolve you can use these metallic hydroxides to consume excess nitric and get a higher Pd concentration. Filter the solid Pt/Au metallics out and melt them. To the solution containing the Pd in nitrate medium you have a few options, most all of which involve ion exchange. You'd probably be best served in the end by taking all of the close cut pieces with the values on it and melting them into a bar and selling them to a refinery.



If you find this useful, please consider making a donation to the gold refining forum.


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## zwai (Apr 16, 2016)

nickvc said:


> If they are old eastern block telephone equipment they are normally very high yielding for gold and PGMs from what I have seen, the PGMs will be either small dots or dashes on some of the relays, if there are switches check them also, in fact test all places where the use of precious metals could be an advantage even if only a small one.
> The newer Nokia material I'm sure others can help with identifying where the best material is to be found, be aware of collectors values on older equipment sometimes it pays better to sell items rather than refine them.
> 
> The ph of your nitric solution will make no difference to forming silver chloride and while the Pd will go into solution any Pt alloys will remain as solid pieces, Pt and Rh are not keen to dissolve even in hot Aqua Regia so perhaps once you have dissolved the base metals and Pd filter the solution and recover the Pt from the filter paper.
> If you wish to refine your PGMs make sure you know what your doing as I have said before they produce some very toxic salts, also to get high quality you need clean saturated solutions to precipitate the salts from so you Amy have to process them several times.




Thanks Nickvc

These servers came from Finland. I do not now how old is land line but Nokia is made in 1995 ( checked from relays codes ). Land line should be from 70 as there where some documents. 

Gold content is very low as pins are made with palladium. Gold seems to be used " just in case". Relays have some gold dots but if I recovered them, Only thing I got was flakes of gold so I leaved them for another time. I certainly run small test of all parts from this server to find out if there is some values.

At the moment I try to recover larger peaces as circuit boards and plates. Plates have solder on them, is it best to wash them with HCl before adding nitric acid to dissolve palladium/copper/etc? If I cement with copper do tin cement as well?

Yes as I recover palladium from aqua regia with DMG it seems that lot of salts and work for small quantity of palladium. 

I add copper and bubbler to my Pd solution and waiting for results. I add some heat and hoe it help to accelerate process.

Thank you for helping out!


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## zwai (Apr 16, 2016)

Lou said:


> I've done a lot of those little fella's. There should be no silver.
> 
> Addressing your present situation--use fresh metallic material (feedstock) to cement out or reduce the mess you have, check to be sure the Pd is removed, filter all that lot of material. You can basically use these metallics over and over to concentrate the Pd before melting and granulating to re-dissolve.
> 
> ...



Hello Lou,

thank you for useful information!

I used only small quantity of material but I surely recover mess I did. Now I will use only copper to cement Pd out. I just need that recovered Pd is 30% clean so I can sell it.

About donation, How can I do it? I definitely want to give my part to Goldrefiningforum as it helped me a lot on this 3 year journey and it bring to me this opportunity to recover these servers.
Please let me know how I can make donation.

Regards


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## zwai (Apr 16, 2016)

UncleBenBen said:


> zwai said:
> 
> 
> > Only problem is Ni ... is it cementing with palladium if I add copper plate to solution?
> ...




Thank you UncleBenBen

I just suspected that copper will drag down all materials as Zinc. I will use copper then. How much heat is max for this recovery?

Thank you for info!


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## FrugalRefiner (Apr 16, 2016)

zwai said:


> About donation, How can I do it? I definitely want to give my part to Goldrefiningforum as it helped me a lot on this 3 year journey and it bring to me this opportunity to recover these servers.
> Please let me know how I can make donation.


Take a look at the recent thread, Donations?.

Dave


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## zwai (Apr 16, 2016)

FrugalRefiner said:


> zwai said:
> 
> 
> > About donation, How can I do it? I definitely want to give my part to Goldrefiningforum as it helped me a lot on this 3 year journey and it bring to me this opportunity to recover these servers.
> ...




Thanks for information Dave!


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## Deon1 (Jun 7, 2019)

What does DMG stand for and what is it. If someone can tell me please


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## anachronism (Jun 7, 2019)

Deon1 said:


> What does DMG stand for and what is it. If someone can tell me please



Sure no problem Deon it's Dimethylglyoxime


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## FrugalRefiner (Jun 7, 2019)

You'll find a lot of terms like this in A Glossary of Common Terms in The Library.

Dave


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