Refining MLCC´s for Palladium and Silver !

[kurtak]

As an update to this thread & the OP

Lars & I have been in a private discussion the last few days

Based on pics Lars posted in this thread it "looked" like maybe he was doing this in an (his) apartment (not a good thing) - so that was my first question

As it turns out - it's being done in a "dedicated" room at his place of work - so good news there

However - the room the work is being done in is under "positive" air pressure (not so good)

So - currently - I am instructing him on how to build a quick & cheap fume hood that will put the room under "negative" air pressure - before we move forward with doing any more work in this room &/or on this project

All chems, solutions & solids are currently in closed containers & will be remaining that way until we get the room under negative air pressure - at which point we will go back to working on the recovery of his values

Kurt

 

[kurtak]

And there are no such thing as 55% HCl, concentrated HCl is around 38%.

That is correct - so he does NOT need to dilute it & as a "matter of fact" do NOT dilute it !!!

Throw away any magnetic MLCCs. They are nickel, no PMs in them.

You beat me to it

It is a waste of chem as well as time to process the magnetic ones --- there is little or NO value in them - they are made with an alloy of nickel & copper - the nickel is what makes them magnetic

Kurt

 

[dpgold]

You quoted Ohiogoldfever!
And there are no such thing as 55% HCl, concentrated HCl is around 38%.
You only need to dissolve Tin until it can’t dissolve more. Make sure there are some left.

Throw away any magnetic MLCCs. They are nickel, no PMs in them.
Grind the remaining to a fine powder and leach in Nitric.
It will dissolve both Ag and Pd.

Thanks, yes that's what it says on the recipient, industrial 55 percent HCL.....

 

[Yggdrasil]

Thanks, yes that's what it says on the recipient, industrial 55 percent HCL.....

I do not think you can get stronger than 38% unless you have pressurized conditions.
And then we are talking Scientific lab conditions.
Can you post images of the label of your acid?
Read here: Hydrochloric acid - Wikipedia

 

[dpgold]

Yes I made a mistake is 32 percent technical grade, I have identical containers for nitric which is 55 percent, the HCL is 32 percent. I was convinced it was this one

 

[Geo]

You quoted Ohiogoldfever!
And there are no such thing as 55% HCl, concentrated HCl is around 38%.
You only need to dissolve Tin until it can’t dissolve more. Make sure there are some left.

Throw away any magnetic MLCCs. They are nickel, no PMs in them.
Grind the remaining to a fine powder and leach in Nitric.
It will dissolve both Ag and Pd.

Actually, there is higher concentrations of HCl but usually not for sale to the general public. Higher than 36% has to be stored under pressure.

 

[Yggdrasil]

Actually, there is higher concentrations of HCl but usually not for sale to the general public. Higher than 36% has to be stored under pressure.

See my post two steps up

 

[dpgold]

See my post two steps up

yes thank you, I read it, as I said I made a confusion and remembered the numbers of concentration from the nitric acid which had 55 percent on it, it was not the HCL which in fact had 32 percent. It was just a mix of numbers in my mind, that is all.

 

[jphayesjr]

Please, could you post pictures of these items?

 

[jphayesjr]

Hope this glass ampule in line reed image helps. There's also a boxy type from Schneider for trucks, ceramic chip types for industry and aerospace. Soviet era military equipment is another source.

 

[MicheleM]

Thank you. Absolutely beautiful, the picture is low resolution but I can see the plated part clearly, it doesn't look have Hg, i would guess N2 gas. I hope for Rhodium! I don't know if i can help but this is what I did with Reed relays:
1) brief research online for the gas filler of each different kind of Reed relays
2) (if not Hg) i broke the glass far from the center to avoid damage to the plated part.
3) for each kind of Reed I cut the base metal near the plated part and i recovered the foils using CuCl2 (not HCl+H202). Don't put them all together because some could have Ruthenium or tungsten plated part. Take a single foil of each kind of reed and test them In a tube with just a little quantity of bleach to identify possible Ruthenium (Ruthenium will react visibly). if no reaction, rinse with water and then test with H2O2, if strong reaction and yellow residue than the foil is made of tungsten. If no reaction of weak reaction with H202, it could be Rhodium or white Gold alloy with high probability

 

[Ohiogoldfever]

I have a nice pile of these read switches. Seems a guy could just scrape the tips into something to avoid digesting tons of un needed materials.

Or clip the tips off and toss the rest.

 

[jphayesjr]

Thank you. Absolutely beautiful, the picture is low resolution but I can see the plated part clearly, it doesn't look have Hg, i would guess N2 gas. I hope for Rhodium! I don't know if i can help but this is what I did with Reed relays:
1) brief research online for the gas filler of each different kind of Reed relays
2) (if not Hg) i broke the glass far from the center to avoid damage to the plated part.
3) for each kind of Reed I cut the base metal near the plated part and i recovered the foils using CuCl2 (not HCl+H202). Don't put them all together because some could have Ruthenium or tungsten plated part. Take a single foil of each kind of reed and test them In a tube with just a little quantity of bleach to identify possible Ruthenium (Ruthenium will react visibly). if no reaction, rinse with water and then test with H2O2, if strong reaction and yellow residue than the foil is made of tungsten. If no reaction of weak reaction with H202, it could be Rhodium or white Gold alloy with high probability

This is a recent photo of a currently manufactured item from Littelfuse. Reference price in 2020 was $2317. The elements are solid rhodium fused to silver-palladium around the twist at the base. Glad it's helpful.

 

[jphayesjr]

Another type containing rhodium, plate or a tiny patch at contact surface approx $60 msrp

DAR71210F-HR - Reed Relay, Rhodium, SPST-NO, 12 VDC, D-HR Series, Through Hole, 150 ohm, 3 A, Cynergy brand​

 

[MicheleM]

Very good stuff!!! Congratulations

 

[B-Rock905]

What we have here is a dead man. His body just does not know it yet. Despite protestations otherwise, all images provided showing hands demonstrate no safety considerations of any kind.

An enclosed room with ventilation is NOT a safe environment to perform what you are doing. Handling contaminated glassware without proper protection can easily allow toxic metal salts to enter the body, causing vital organs such as kidneys, liver, and lungs to fail in a few months to a few years. Yes, just one exposure can do this.

Get you mind right. Put your toys away. Read the entire section on Safety. EVERY THREAD. At least three times. Come back when you have an understanding of the potential hazards of what you are working with.

Time for more coffee.

No Doubt about it! Even after being asked to do it, this fellow is in such a Rush to the Goal line that he has completely Swapped Safety First for insanity! Here's the thing, we all made mistakes when we first started to learn about basic and or advanced chemistry. But there were 2 differing sides just as Volatile as Political Parties. There were some, who learned from some help of a Chemist or Chemical Management course. You know, the knowledge Gleaned from person to person learning. Or the other side who watch a Bogus YouTube Video on how to Recover gold from a ore Sample by simply Soaking the Sample in Red Cider Vinegar, then transfer all of the Ore and liquid into a 8 quart bowl and then Quickly Covering the contents of the Bowl with a large 1-2 cup scoop of Sodium Bicarbonate. And Walla! No Gold, just a Huge mess! No thanks I'll stick with one on one or a peer type learning environment.

 

[willworld.whr]

I know I have more studying to do myself, thus I'm in no hurry until I'm confident with exactly what steps In process I'm going to preform. My question is what is the reason behind telling him not to let it dry or be subjected to light?

 

[Rreyes097]

As long as the MLCC's remain whole, there will be metal left to reclaim. Most people mill or crush them before starting. I don't like milling. It creates too much fine silt that the acid has to struggle to get through unless you have an overhead stirrer. When wet processing, the ceramic bodies have to break down into dust to get a complete leaching. They will break down in the acid by just heating. The bodies are sintered alumina ceramic. They will slowly come apart during the leaching. I find it's better to put an excess of solution in the beaker with the MLCC's and cover and place on heat and forget about it until the evening. It normally takes several days to break down all of the bodies. Unless they are crushed before hand. It's best to avoid chlorine during the nitric acid leach if you want to recover the silver. If silver chloride is formed in the alumina powder, there is no good way to separate the two again. It's just trash. Actually it's best not to introduce HCl to the process at all until all of the nitric acid leaches are complete and filtered. Then add HCl to remove the silver. Or dissolve some non-iodized table salt in water and pour that into the silver nitrate. It has the same effect that HCl does but is much less expensive. Using AR to leach a catalytic metal is a fight against itself. Catalytic metal breaks NO2 down to it's individual atoms. It will dissolve over time but just plain nitric acid works better for me.

What about cementation with copper so you don't have to process silver chloride to silver oxide? Or is it nitrate? Oxide I think. But wouldn't that keep the process shorter? Or is it because you don't want the Pd to cement at the same time?

 

[Yggdrasil]

What about cementation with copper so you don't have to process silver chloride to silver oxide? Or is it nitrate? Oxide I think. But wouldn't that keep the process shorter? Or is it because you don't want the Pd to cement at the same time?

That means you already have milled and dissolved them in Nitric.
Wet processing are not effective.

Anything you cement is going to be metallic.

If you convert to Silver Chloride, you can convert it to Silver Oxide and then Silver.
Or use Iron/Sulfuric method or smelt…

Maybe study a bit more?

 

[Rreyes097]

That means you already have milled and dissolved them in Nitric.
Wet processing are not effective.

Anything you cement is going to be metallic.

If you convert to Silver Chloride, you can convert it to Silver Oxide and then Silver.
Or use Iron/Sulfuric method or smelt…

Maybe study a bit more?

I'm familiar with the process of converting silver chloride to silver oxide. I have successfully performed it many times now. I was just wondering why not cement on copper instead of dropping silver chloride with HCL? But I think I know the answer. It's so you can next instead cement the Pd, if any, via copper cementation. Am I correct? And what do you mean I have milled and dissolved in nitric? Me? Have I milled? No. Have I dissolved in nitric? Yes, but the mlccs are not much dissolved much at all. So all are in the same shape more or less. But I'm currently working on a test batch of 20g. So this is me studying more. I'm learning the process on a small sample size as directed by forum members. Read, research forum, ask questions, videos. My research has shown me that sample sizes are the way to go. So thats what I'm doing. I've spent all day reading this stuff. Which can be quite difficult to a non chemistry mind or background. So terms and base knowledge I'm gathering as I learn. But I've been studying literally all day.