Palladium in solution? Help I'm new

[Smithy]

Let me start by saying thank you. This is my first post, but I've been haunting this site for many months. Lots of great information here. I am new to silver refining. I have watched almost all of streetips videos on the subject and made a silver cell very similar to his (only smaller 2.5 liters). My cell is running good, but i ran into a problem today and I can't seem to find the answer anywhere. I just dissolved 890 grams of silver spoons in nitric and my solution is green. I am pretty sure its palladium in solution. I just need confirmation and a question answered. I did a stannous test with solution I made from 95/5 tin/antimony dissolved in hydrochloric acid. My question then is, if it is Palladium, do I need to precipitate it out with DMG before I cement the silver out? Or can I just cement everything out on copper, and then run it through the silver cell? The stannous test looks like silver chloride with palladium. I know you can catch the palladium in the silver cell filters, but will this cause any problems clogging my filters up? I have attached a picture of my solution and my stannous test. Any help would be greatly appreciated!

 

[MicheleM]

Why are you sure palladium should be in solution?
Maybe the picture has too low resolution but I do not see any green color in your stannous test that confirm Pd in solution

 

[Smithy]

It is my understanding, that palladium will show up brown with stannous test when dissolved with sterling silver. If not palladium, what could it be? I have a lot to learn. Here is a shot of what my solution normally looks like under the same light.

 

[MicheleM]

I can only say that the solution is heavily contaminated with base metals, it doesn't look a silver nitrate solution, by far. Anyway the original question remains: why do you think Pd should be in solution? Comment 4 of
https://goldrefiningforum.com/threads/stannous-test-result-identification.31288/#post-329204

 

[Smithy]

I’ve been researching this all day and came across a video of streetips refining the silver cell filter slimes. The solution looked about the same color and the stannous was coming up brown, just like mine. I’m drawing my conclusion based on that. This is why I decided to post. I’m not sure. If it is base metal contamination, the silver should cement out as usual right? I just might not have the yield I was expecting I would assume.

 

[MicheleM]

This will be my last answer because you didn't respond to my question at all. Anyway a Silver nitrate solution is nearly colorless, that means that your solution, looking to the second picture, is heavily contaminated with base metals. If you have used enough nitric both silver and base metal can stay in the same solution, do you want to see silver? You can use a copper bar to cement it out, note that you need to react with almost all the free nitric. Good luck

*Edit for clarification: even if Pd can also show brown in stannous for low concentration, i have seen too many brown false positive so that first question is: why should Pd be in your solution ?

 

[nickvc]

To add to what is now the active point
Why do you expect to find palladium in your solution?
Sreetips processes lots of jewellery including white gold which can and does have palladium in it so when inquarting his scrap and processing in nitric the palladium and other PGMs will follow the silver into solution , once the solution is cemented the PGMs will again follow the silver back out of solution if done correctly which will then be added to his cell hence the palladium.
You are processing spoons so why would you expect palladium?
Same question as has been asked many times now.

There seems to be a preoccupation with palladium in many youtube videos even when they are processing e scrap but unless you are processing phone scrap or certain specific types of scrap you are not likely to encounter it, if you process jewelry then yes but e scrap very unlikely.

 

[snail]

Cement as usual. Early in my refining I ran into high quality silver palladium contacts. The solution didn’t look very different from normal, but near the end of cementation it turned green. That was the clue.

If it exists it will report to the slimes and solution. If present the solution often gets a slight greenish cast. That is the time to deal with it.

 

[Yggdrasil]

Let me start by saying thank you. This is my first post, but I've been haunting this site for many months. Lots of great information here. I am new to silver refining. I have watched almost all of streetips videos on the subject and made a silver cell very similar to his (only smaller 2.5 liters). My cell is running good, but i ran into a problem today and I can't seem to find the answer anywhere. I just dissolved 890 grams of silver spoons in nitric and my solution is green. I am pretty sure its palladium in solution. I just need confirmation and a question answered. I did a stannous test with solution I made from 95/5 tin/antimony dissolved in hydrochloric acid. My question then is, if it is Palladium, do I need to precipitate it out with DMG before I cement the silver out? Or can I just cement everything out on copper, and then run it through the silver cell? The stannous test looks like silver chloride with palladium. I know you can catch the palladium in the silver cell filters, but will this cause any problems clogging my filters up? I have attached a picture of my solution and my stannous test. Any help would be greatly appreciated!

What kind of Silver spoons?
Sterling, 830s or what.
Under normal circumstances there will not be Pd in there.
It is hard to tell what colors can come from mixed Nitrate base metal salts.
The stannous looks more like the false positives we see from time to time.

 

[FrugalRefiner]

It is possible to encounter minor amounts of palladium in old silver flatware, old being the key word. Back then, refining techniques weren't quite as good as they were now, and palladium wasn't nearly as valuable as it is now, so refiners didn't worry about a tiny amount staying with the silver.

Cement your silver out as usual. The palladium will cement out with it. When you run it through your silver cell, the palladium will dissolve into your electrolyte along with the silver, but if you have your cell set up right, the palladium will remain in the solution as long as the concentration doesn't rise too high.

Dave

 

[kurtak]

the stannous was coming up brown

You can NOT trust a stannous on silver nitrate !!!

Why ?

Because when you add the stannous - which is HCl - to the silver nitrate the HCl in the stannous converts some of the silver nitrate to silver chloride

The silver chloride which is the exposed to light then does what is called photo greying - which happens very quickly

Though it is called photo greying the silver chloride can change color from normal silver chloride white to grey - black - purple - or brown --- depending on type of light exposer - amount of light exposure time - concentration of silver in solution - &/or other base metals in the solution

Photo greying is the principle behind using silver compounds for developing black & white photographs

All silver compounds photo grey --- it why if you get silver nitrate on your hand - spill it on your lab counter top - don't wash it all out of your filter paper it will photo grey to one of the above colors

That is why you can NOT trust a stannous test on silver nitrate --- it IS going to photo grey & give you a FALSE positive !!!

Therefore - IF (the BIG IF) you suspect Pd in your silver nitrate you MUST do a DMG test on the silver nitrate

That test is done by putting 3 or 4 drops of silver nitrate in a test tube (or plastic spoon) & adding 1 drop of DMG solution --- if Pd is in solution it will precipitate the yellow DMG/Ag salt

Kurt

 

[kurtak]

I just dissolved 890 grams of silver spoons in nitric and my solution is green.

The color of your solution (first pic first post) does not look green to me but looks blue which is clearly copper in the silver nitrate

It is just a lighter blue then your second pic (different/normal solution) because ether there was less copper in the silver then normal - or the lighter (blue) solution is more dilute then normal

I have had batches of OLD silverware that were 975 instead of the normal 925 & being higher in silver & lower in copper results in a lighter blue solution

One "larger" such batch I did years ago (spoons forks platers bowls etc.) was ether from (made in) China or Japan (don't remember exactly anymore) it was a very old silver set & was 975 silver --- I used some of it to make my electrolyte for my silver cell (because of the low copper in it) & the solution was very light blue

Because of the low copper content the rest of it was melted into anodes & run directly in the silver cell

Edit to add; - my point being that it is possible (though rare) to get silverware that is higher in silver then the normal 925 which will result in a lighter blue solution due to higher silver lower copper

Kurt

 

[Smithy]

This will be my last answer because you didn't respond to my question at all. Anyway a Silver nitrate solution is nearly colorless, that means that your solution, looking to the second picture, is heavily contaminated with base metals. If you have used enough nitric both silver and base metal can stay in the same solution, do you want to see silver? You can use a copper bar to cement it out, note that you need to react with almost all the free nitric. Good luck

*Edit for clarification: even if Pd can also show brown in stannous for low concentration, i have seen too many brown false positive so that first question is: why should Pd be in your solution ?

Thank you for all of your help. You will have to forgive my ignorance. The metal was a batch of spoon bowls. The handles had been snipped off so nothing was marked. I am starting to think I got ripped off on this ebay purchase. I had to throw out about an ounce of the metal during the torching process because I could tell it was plated material. I would bet that some of the other pieces were not sterling. Yes I used up all the free nitric. I thought I answered your question in my last post but I will try to make it very clear. I thought Pd was in the solution because of that video I mentioned in my last reply. Also, through all the research I have done, I know Pd was sometimes used (in older material) used as an alloy in sterling. Since I have no way of dating the spoon bowls, I made the assumption. You are probably correct. It is most likely base metal contamination and I think I will cement the silver out as usual. I will post an update on my final yield if you are interested. Thanks again.

 

[Smithy]

To add to what is now the active point
Why do you expect to find palladium in your solution?
Sreetips processes lots of jewellery including white gold which can and does have palladium in it so when inquarting his scrap and processing in nitric the palladium and other PGMs will follow the silver into solution , once the solution is cemented the PGMs will again follow the silver back out of solution if done correctly which will then be added to his cell hence the palladium.
You are processing spoons so why would you expect palladium?
Same question as has been asked many times now.

There seems to be a preoccupation with palladium in many youtube videos even when they are processing e scrap but unless you are processing phone scrap or certain specific types of scrap you are not likely to encounter it, if you process jewelry then yes but e scrap very unlikely.

Yes, you are probably right. Good point about the difference in material we are processing. I will have to admit, I didn't really think about that. The material was a batch of sterling spoon bowls I purchased on ebay. I have learned that they sometimes used Pd as an alloy in sterling, but now that I'm thinking about it, the amounts would probably be too small for me to even notice it in my solutions. I think I either got a bad deal on this purchase, or there was a lot more 80% spoons than sterling. All of the material I have processed so far has been a copper alloyed sterling silver. My solutions have all been a bright blue. This is what has me scratching my head at the moment. Thank you for your input. I still have a lot to learn but I am having a lot of fun!

 

[Smithy]

Cement as usual. Early in my refining I ran into high quality silver palladium contacts. The solution didn’t look very different from normal, but near the end of cementation it turned green. That was the clue.

If it exists it will report to the slimes and solution. If present the solution often gets a slight greenish cast. That is the time to deal with it.

Thank You!

 

[Smithy]

You can NOT trust a stannous on silver nitrate !!!

Why ?

Because when you add the stannous - which is HCl - to the silver nitrate the HCl in the stannous converts some of the silver nitrate to silver chloride

The silver chloride which is the exposed to light then does what is called photo greying - which happens very quickly

Though it is called photo greying the silver chloride can change color from normal silver chloride white to grey - black - purple - or brown --- depending on type of light exposer - amount of light exposure time - concentration of silver in solution - &/or other base metals in the solution

Photo greying is the principle behind using silver compounds for developing black & white photographs

All silver compounds photo grey --- it why if you get silver nitrate on your hand - spill it on your lab counter top - don't wash it all out of your filter paper it will photo grey to one of the above colors

That is why you can NOT trust a stannous test on silver nitrate --- it IS going to photo grey & give you a FALSE positive !!!

Therefore - IF (the BIG IF) you suspect Pd in your silver nitrate you MUST do a DMG test on the silver nitrate

That test is done by putting 3 or 4 drops of silver nitrate in a test tube (or plastic spoon) & adding 1 drop of DMG solution --- if Pd is in solution it will precipitate the yellow DMG/Ag salt

Kurt

Thank you! I just learned something new!

 

[Smithy]

Thank you all for your input! I've decided to cement the silver out with copper as usual. I think if there is any Pd in solution, its probably too small to even worry about. Most likely base metal contamination. I will post an update with my final yields in a couple days if anyone is curious.

 

[VK3NHL]

Let me start by saying thank you. This is my first post, but I've been haunting this site for many months. Lots of great information here. I am new to silver refining. I have watched almost all of streetips videos on the subject and made a silver cell very similar to his (only smaller 2.5 liters). My cell is running good, but i ran into a problem today and I can't seem to find the answer anywhere. I just dissolved 890 grams of silver spoons in nitric and my solution is green. I am pretty sure its palladium in solution. I just need confirmation and a question answered. I did a stannous test with solution I made from 95/5 tin/antimony dissolved in hydrochloric acid. My question then is, if it is Palladium, do I need to precipitate it out with DMG before I cement the silver out? Or can I just cement everything out on copper, and then run it through the silver cell? The stannous test looks like silver chloride with palladium. I know you can catch the palladium in the silver cell filters, but will this cause any problems clogging my filters up? I have attached a picture of my solution and my stannous test. Any help would be greatly appreciated!

Looks like copper in your silver nitrate sol.

 

[AyYildiz]

Hello,
I can make silver cells, but there is no such trade in My Country.
What is the purpose of the Silver Cell sale?
For what purpose do people who receive the Silver Cell take it?
How can I learn these subjects?

 

[FrugalRefiner]

A silver cell is an electrolytic refining cell used to purify silver to a high level.

You can learn all about these processes by reading the forum.

Dave