palladium in nitric

[teclu]

Hello everybody,


I have a type of pins with Pd under layer of Au(RFT 1971, east germany made). The base metals are Ni alloy(NiFe).

In nitric these pins form a yellow solution, maybe even little orange(like gold in AR), and after a while the gold foils can float in top, base metals remain untouched.
My question is how i can recover palladium from this solution? The Pd is around a 50grams/1 kilo of pins.

Thanks!

teclu

 

[Oz]

I’m not understanding something here if you have nickel and iron in nitric untouched. Even if you had the exact amount of nitric to dissolve the palladium you would have it cement out on the base metals.

 

[butcher]

I would test a batch with sodium chlorate, look for yellow PPT that changes blue green,
you could also try DMG. as Oz asked you may find your values plated to the remaining base metals.

 

[Oz]

Butcher,

Are you sure about using sodium chlorate in nitric? I have never done that so cannot say from experience. The dimethylglyoxime would be close to quantitative for palladium in a nitric solution however.

 

[butcher]

not from personal expierience, but from studying (several sources) it will PPt from nitric. this is why I suggested testing with. my guess a chloride (or ate) of Pd and a sodium nitrate byproduct but haven't looked into that.

here is a lil bit of info:
http://www.1911encyclopedia.org/Palladium_(Chemistry)

 

[teclu]

I’m not understanding something here if you have nickel and iron in nitric untouched. Even if you had the exact amount of nitric to dissolve the palladium you would have it cement out on the base metals.

Oz,


My nitric acid is 70% and the solution usually I used is the following: 4 ml acid + 4 ml tap water for 1 gram of metal. The RFT connectors pins are magnetic,is true that I do not know exactly the type of base metals alloy but I guess they have much iron in alloy, because after 2 or 3 hours in nitric solution was what I said above: the gold foils were separated and floating, the body of pin (base metal) remained untouched(of stainless steel shade), and the solution took a yellow to orange shade. Also, I know for sure that pins containing palladium deposited in a layer 5 microns,... under gold layer.

Then for palladium, which is the way to recover it from the solution?
Can you please explain in more detail this cementation?

Thanks!

teclu

 

[Harold_V]

Then for palladium, which is the way to recover it from the solution?
Can you please explain in more detail this cementation?

Assuming you don't have excessive nitric present, and assuming you have the palladium in solution, it can be recovered with copper, using the same procedure as for cementing silver. Palladium is slow to cement down, however, and will deposit as a black film. The more surface area you present, the faster will be the cementation process, but it will also require cleaning of more surface area to recover the cemented palladium. If you aren't in a hurry, use a small amount of copper, although a piece, not wire, and allow it to cement. Check the solution periodically with DMG or stannous chloride to determine when it is barren.

I'm not very encouraged by your description of the solution color. It takes very little palladium to turn a solution dark, often the color of coffee. I expect there is very little palladium present.

Harold

 

[teclu]

Then for palladium, which is the way to recover it from the solution?
Can you please explain in more detail this cementation?

Assuming you don't have excessive nitric present, and assuming you have the palladium in solution, it can be recovered with copper, using the same procedure as for cementing silver. Palladium is slow to cement down, however, and will deposit as a black film. The more surface area you present, the faster will be the cementation process, but it will also require cleaning of more surface area to recover the cemented palladium. If you aren't in a hurry, use a small amount of copper, although a piece, not wire, and allow it to cement. Check the solution periodically with DMG or stannous chloride to determine when it is barren.

I'm not very encouraged by your description of the solution color. It takes very little palladium to turn a solution dark, often the color of coffee. I expect there is very little palladium present.

Harold

Sir,

Thank you for your response, I appreciate this punctuality all the time at you.

Now, which is the amount of nitric 70% required to dissolve 1 gram of Pd?
Assuming i have 1 liter of nitric solution(50/50) with dizolvated Pd in, if I use a copper plate or sheet , which is the amount of copper consumed for cementing 1 oz of Pd, and how long is the process of cementing, approximately?
How to wash the black powder?

teclu

 

[Oz]

If you are positive that you have palladium as part of your raw material I think the first thing you need to do is find out where it is with stannic. I’m with Harold that I find it unlikely that you have much if any palladium dissolved in your nitric as palladium nitrate aqueous is brown.

You seem sure that you have removed all precious metals from this material and the remainder is magnetic. I would remove the magnetics and agitate and wash free any residues and recombine the wash with your foils. You would probably have a gold/Pd mix that you could take into AR after filtering or decanting to remove the bulk of the solution. Precipitate your gold then check with stannous for your Pd.

Make sure to check all of your washes and I would take a sample of your pins that were removed magnetically and digest them completely in AR and check with stannous to be sure all values were removed.

 

[teclu]

If you are positive that you have palladium as part of your raw material I think the first thing you need to do is find out where it is with stannic. I’m with Harold that I find it unlikely that you have much if any palladium dissolved in your nitric as palladium nitrate aqueous is brown.

You seem sure that you have removed all precious metals from this material and the remainder is magnetic. I would remove the magnetics and agitate and wash free any residues and recombine the wash with your foils. You would probably have a gold/Pd mix that you could take into AR after filtering or decanting to remove the bulk of the solution. Precipitate your gold then check with stannous for your Pd.

Make sure to check all of your washes and I would take a sample of your pins that were removed magnetically and digest them completely in AR and check with stannous to be sure all values were removed.

Oz,

I admit that I do not know so well to read the test results for Pd, with stanous chloride, and DMG i have not yet, but tomorrow will dissolve in nitric a piece of Pd 99%, (a cursor of a russian potentiometer) and after that I will compare the solutions colours...someone even said that Pd can be sometimes chameleon.

Until then remains to thank you for your reply and for your indications, I apreciate it.

teclu

 

[Palladium]

I admit that I do not know so well to read the test results for Pd, with stanous chloride, and DMG i have not yet, but tomorrow will dissolve in nitric a piece of Pd 99%, (a cursor of a russian potentiometer) and after that I will compare the solutions colours...someone even said that Pd can be sometimes chameleon.

Until then remains to thank you for your reply and for your indications, I apreciate it.

teclu

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=1692&start=20

http://goldrefiningforum.com/phpBB3/viewtopic.php?t=646&start=0&postdays=0&postorder=asc&highlight=

Somewhere in forum book 1 or 2 it shows the results ( different colors ) of Stanous tests.

 

[teclu]

I admit that I do not know so well to read the test results for Pd, with stanous chloride, and DMG i have not yet, but tomorrow will dissolve in nitric a piece of Pd 99%, (a cursor of a russian potentiometer) and after that I will compare the solutions colours...someone even said that Pd can be sometimes chameleon.

Until then remains to thank you for your reply and for your indications, I apreciate it.

teclu

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=1692&start=20

http://goldrefiningforum.com/phpBB3/viewtopic.php?t=646&start=0&postdays=0&postorder=asc&highlight=

Somewhere in forum book 1 or 2 it shows the results ( different colors ) of Stanous tests.

Palladium,

Thanks for the links, in fact the real problem for me is not stanous chloride test for Pd, but how I manage to recover Pd from nitric solution.

teclu

 

[lazersteve]

To recover the palladium you can evaporate the solution down to a dark red syrup (dark like wine) then add HCl. Repeat this process three times or until no more brown fumes are produced when the HCl is added.

Perform this in a well ventilated area as the brown fumes are deadly to breath.

Once the palladium nitrate is converted to palladium chloride you can add ammonium chloride followed by small amounts of sodium chlorate to the hot solution to precipitate the palladium.

I demonstrate the precipitation process on my Platinum and Palladium DVD.

Steve

 

[Harold_V]

Now, which is the amount of nitric 70% required to dissolve 1 gram of Pd?

Unfortunately, I am unable to answer that question. Were it my problem, I'd introduce a small amount and see how far it goes. You can then judge how much would be required. Others on the forum have the math skills and knowledge to answer your question directly.

Assuming i have 1 liter of nitric solution(50/50) with dizolvated Pd in, if I use a copper plate or sheet , which is the amount of copper consumed for cementing 1 oz of Pd, and how long is the process of cementing, approximately?

The amount of copper that would be consumed would not be extreme, but, again, I am unable to answer that question. I simply don't know.

As far as the time required, as I mentioned, the more surface area you provide, the faster it will cement. Providing even a vague answer wouldn't be prudent. You should be able to recover all of your palladium in a full day, assuming you use a reasonable amount of copper.

It is VERY important that you be able to judge what you have in solution, otherwise you may be wasting your time. Test the solution with stannous chloride, or if you have doubts about the results, use DMG. With DMG, the test will result in a brilliant yellow precipitate if you have any palladium present. It is a very sensitive test, so even traces of palladium will yield a visible amount of the precipitate.

How to wash the black powder?

I would not consider the recovered powder as having been refined, only recovered. Palladium, unlike gold, will NOT precipitate from a dilute solution. That's why I suggested you recover it with copper. I would rinse the recovered black powder well with water, dry it and then store it for the day when I had enough to re-process. I would then dissolve it in nitric, evaporate, filter, then precipitate using ammonium chloride and sodium chlorate. It is done hot, not cold. Read Hoke for clarification.

Hope this helps.

Harold

 

[SapunovDmitry]

My analysis shows 0,3-0,5% of Pd on RFT pins.
Are you talking about flat "knifelike" pins in black plastics, where it says RFT TGL 10395 AuPd?
Or maybe we are talking about different types of pins?
What is the gold content of these pins?
My shows 0,55-0,85 % by weight.

 

[teclu]

Now, which is the amount of nitric 70% required to dissolve 1 gram of Pd?

Unfortunately, I am unable to answer that question. Were it my problem, I'd introduce a small amount and see how far it goes. You can then judge how much would be required. Others on the forum have the math skills and knowledge to answer your question directly.

Assuming i have 1 liter of nitric solution(50/50) with dizolvated Pd in, if I use a copper plate or sheet , which is the amount of copper consumed for cementing 1 oz of Pd, and how long is the process of cementing, approximately?

The amount of copper that would be consumed would not be extreme, but, again, I am unable to answer that question. I simply don't know.

As far as the time required, as I mentioned, the more surface area you provide, the faster it will cement. Providing even a vague answer wouldn't be prudent. You should be able to recover all of your palladium in a full day, assuming you use a reasonable amount of copper.

It is VERY important that you be able to judge what you have in solution, otherwise you may be wasting your time. Test the solution with stannous chloride, or if you have doubts about the results, use DMG. With DMG, the test will result in a brilliant yellow precipitate if you have any palladium present. It is a very sensitive test, so even traces of palladium will yield a visible amount of the precipitate.

How to wash the black powder?

I would not consider the recovered powder as having been refined, only recovered. Palladium, unlike gold, will NOT precipitate from a dilute solution. That's why I suggested you recover it with copper. I would rinse the recovered black powder well with water, dry it and then store it for the day when I had enough to re-process. I would then dissolve it in nitric, evaporate, filter, then precipitate using ammonium chloride and sodium chlorate. It is done hot, not cold. Read Hoke for clarification.

Hope this helps.

Harold

Sir,

Many thanks, I hope I understood enough, no doubt that I will use your teachings and Hoke's also.

teclu

To recover the palladium you can evaporate the solution down to a dark red syrup (dark like wine) then add HCl. Repeat this process three times or until no more brown fumes are produced when the HCl is added.

Perform this in a well ventilated area as the brown fumes are deadly to breath.

Once the palladium nitrate is converted to palladium chloride you can add ammonium chloride followed by small amounts of sodium chlorate to the hot solution to precipitate the palladium.

I demonstrate the precipitation process on my Platinum and Palladium DVD.

Steve

Steve,


I appreciate very much your help, always.
Thank you!

My analysis shows 0,3-0,5% of Pd on RFT pins.
Are you talking about flat "knifelike" pins in black plastics, where it says RFT TGL 10395 AuPd?
Or maybe we are talking about different types of pins?
What is the gold content of these pins?
My shows 0,55-0,85 % by weight.

Hello,

Here are two types of male RFT connectors and another russian.
http://i30.tinypic.com/5lxu9y.jpg
http://i31.tinypic.com/1zkx8pj.jpg
http://i32.tinypic.com/3306deq.jpg

At the RFT connectors only samples I processed at the moment, from 20 grams of RFT pins completely gold plated, resulted 280 mg of foils.
From 1 kilo of russian male pins resulted 43 grams of brown powder.

Please help me understand, what you say is that from 1kg of RFT pins result only maximum 5 grams of Pd?
Please tell me which is your procedure for Pd, you have a picture with your connectors?
If it proves true then not really worth the lost time with Pd.
Thanks in advance!

teclu

 

[SapunovDmitry]

According to my assay book those russian pins have 3,7-4 % per weight of pins gold content.
Have you ever seen russian female pins that have "РПМ23-......." marking?
If so what was your yield on those ones))).
My assay says that it is 75 grams of Au per kg of female pins.
I've never seen those RFT pins you've posted. I was talking about other type of larger male pins, so i am not saying that you don't have 1-3 % of Pd in them. I will post pictures as soon as i get to the lab.

 

[teclu]

According to my assay book those russian pins have 3,7-4 % per weight of pins gold content.
Have you ever seen russian female pins that have "РПМ23-......." marking?
If so what was your yield on those ones))).
My assay says that it is 75 grams of Au per kg of female pins.
I've never seen those RFT pins you've posted. I was talking about other type of larger male pins, so i am not saying that you don't have 1-3 % of Pd in them. I will post pictures as soon as i get to the lab.

I have not this female connector yet(military type I guess), but in the catalog this female РПМ23-32Г5 with 32 of pins, contains 0,399 grams of Au(12 mg of Au/1 pin). If the weight of pins(with base metals)/1 connector is around 5,3 grams then your 7,5% percent is corect. Anyway your percent can be corect because exist the russian military connectors with more than 7,5% Au/kg of pins.

My russian connectors(from the picture above) have 96 pins and the content(after same catalog) is 0,290 grams/male connector and 0,420 grams /female connector.The weight(with base metals) of male pins/1 connector is 6 grams and for female is 12 grams, the percents are 4,8% for male and 3,4% for female.From 1kg of male pins my results are 45 grams of brown powder and for female 31,5 grams.

Have you processed the russian ceramic capacitors KM type, with Pt and Pd content?

teclu

 

[arthur kierski]

here in brazil,as we are not aloud to use naclo3,we have a very eficient and easy method to extract the pd from nitric solutions------to the nitric solution we add clorox which makes the solution red(collor) and then we add nh4cl powder and stirr the solution and beautifull pd red salt is formed----note:first clorox and then nh4cl----if one change the order ,an explosion might happens

 

[teclu]

here in brazil,as we are not aloud to use naclo3,we have a very eficient and easy method to extract the pd from nitric solutions------to the nitric solution we add clorox which makes the solution red(collor) and then we add nh4cl powder and stirr the solution and beautifull pd red salt is formed----note:first clorox and then nh4cl----if one change the order ,an explosion might happens

Arthur hello,

Can you tell me please, which are the proportions that you use, I mean the quantities and the tehchnical grade for clorox respectively of NH4CL for 1 liter of nitric solution consumed (of course, nitric solution with Pd)?


Thanks in advance!

teclu