# Recovering silver and palladium from MLCC:s



## g_axelsson

This is a description of how I'm doing silver and palladium recovery from MLCC:s. It is based on various procedures here on the forum, put together in a mix that suits me with the limitations I have in my access to chemicals and the fact that I can't incinerate without a whole lot of work.

As I like to do some experimenting myself and not just follow a receipt that wouldn't suit my situation, I have read a lot about palladium recovery and refining during the winter. Then I put together a procedure that should work for me, given my circumstances. It might differ from common procedure and I'm in the middle of testing it out, but so far so good...

I started with a batch of 145g mixed MLCC:s and I wanted to recover silver and palladium powder for later refining. This is the steps I took. I'm not in a hurry so I can do one step, put it away for a while and then continue weeks later if so. Most steps are not time critical and even benefits from being left alone for some time to let the chemicals react to the end.

Any solutions that were filtered off were checked for values before proper disposal. Any reaction that gives off fumes were done outside. Safety precaution should always be in place when working with strong acids and bases, the pictures are taken outside of the plastic bin I normally use as a catch basin.

1. Soak the MLCC:s in hydrochloric acid to remove tin, lead and other base metals. As I didn't heat it I just left it in acid for several days before switching to new acid. Stopped it when it seemed there were no more reaction. Eventually many of the MLCC:s breaks up into separate metallic foils but it can take a week or longer.
2. Wash and decant the broken down MLCC:s with water to get the chlorides and HCl out, quite some foils in it.
3. Add NaOH to transform any AgCl that formed in the HCl treatment into Ag2O. I don't know if this is necessary or even works.
4. Wash and decant off the NaOH solution
5. Add nitric acid to dissolve the silver, silver oxide and palladium. Some chlorides will remain but they get locked up in silver chloride that forms.
6. Filter off the dissolved values. I decanted and filtered. It was apparent that there were some silver chloride in the reaction vessel as the filter clogged up with silver chloride that turned purple.
7. add NaCl solution to the filtered tea colored solution, it precipitates the silver as white silver chloride. Stop when additional NaCl doesn't make any precipitation.
8. Decant and filter off the palladium solution, I reused the filter from above as it caught all silver chloride. Multiple washes was used to get most of the palladium out from the silver chloride.
9. Treat the silver chloride with NaOH and sugar to get silver powder.
10. Add zinc shavings to the palladium solution to cement out the palladium.
11. Decant off the liquid from the cemented palladium and then wash it with HCl to remove excess zinc and eventual base metals that the zinc precipitated.
... collect, dry and weigh the result. The fluids goes to the proper stockpot and the metal powders are put into respective storage beaker with other powders awaiting final refining when I have enough to do it.

Right now I'm at step 9 and 10.

Some pictures....

Step 5, leaching palladium out of MLCC:s



Step 7, NaCl added and the silver chloride drops to the bottom. The palladium solution is coloring it yellow.



Step 8, decanting the palladium solution from the silver chloride. Pour along a glass rod for better control of the liquid.



Step 8, after two washes. There is still some palladium mixed in with the silver chloride but it is getting paler. I think I made five washes totally.
The minute amount of palladium I didn't wash out will follow the silver until it is separated in the silver cell I'm going to build some day.


Between step 8 and 10, the filtered palladium solution, free from silver.



(Continued below)


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## g_axelsson

Step 10, added zinc turnings. It was like a palladium lava lamp, small bits bobbing up and down. As I had a density gradient from the different washes, many pieces jumped up half ways to the surface and got stuck in the middle, just hovering. 8)



Step 10, almost done now. Just a little more zinc to add.



As this is my first run, there are a lot of things I will improve for the second run, things to note.
- Crushing speeds up the leaching process quite a bit. Maybe I'll try that on the next batch.
- I used too little nitric at first so I'm leaching the solids again and by the color it looks like I'm getting as much palladium in the second leach as the first.
- I'll try to get proper filter paper and a vacuum filtration unit, that ought to speed up filtering and washing the silver chloride.
- My homemade filter holder (a bent copper wire) was attacked by the fumes from the acid and shed some copper scale that dropped in among the palladium. Better make one out of plastic.

Harold, I actually took up Hooks book yesterday and read everything about precipitating palladium from solutions. All involved one or another chloride compound so it wouldn't work with my silver and palladium nitrate solution until after getting the silver out first. I just prefer my solution, collecting cemented metals for the time being.

Comments?

Göran


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## 9kuuby9

from step 10; you could have added FeS04 to participate the Pd from the nitrate solution; and then you can refine it from their.


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## g_axelsson

I haven't heard that copperas, FeSO4, could precipitate palladium. On the contrary, copperas is used to precipitate gold from palladium containing liquids.

In http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=37&t=1438


Harold_V said:


> ....
> In your example, you'd have gold and palladium remaining to be recovered. Assuming you had a large percentage of gold, with a small amount of palladium, you'd selectively precipitate the gold, using one of many precipitants. I used SO2, and also copperas (ferrous sulfate). Each of them will precipitate only the gold, but you'd get considerable drag down of both palladium and copper, so the gold wouldn't end up pure, although very close.
> ....



Do you have a reference of the contrary or is it that FeSO4 could precipitate palladium from nitrate solutions?

By the way, in step 10 it isn't any longer a clean nitric solution, it is a weak aqua regia as I added an excess of NaCl to get the silver out of solution.

Göran


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## g_axelsson

Found it!

http://www.goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=6026&p=87562#p87562

FeSO4 is precipitating palladium from a nitric solution. So are SO2 too, so SMB should also work.
If it works then I could drop the palladium first before going after the silver.

So.... after extracting and filtering the silver palladium leach from the MLCC:s I can do:
- Add SMB to drop palladium as metal
- Decant and filter
- add solid copper to extract silver and trace amounts of other precious metals

This is perfect, I don't have to mess around with silver chloride or palladium salts just to recover a concentrate.

Thanks!

Göran


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## 9kuuby9

I'm glad to help you out. I know that participating gold with SMB or Copperas in a chloride solution causes PGM's drag down. In a nitrate solution it can fully precipitate Pd.

The best way of recovery is to use efficient methods in recovering various metals;

You can crush the MLCC's which is time consuming but it will leach faster and have better yield results.

I first tend to use nitric 50/50 D. water to leach the base metals including Ag & Pd; after 2 or 3 leaches of fresh nitric solution; filter the solids out including the metastannic acid.

Drop out the Pd in the filtered nitrate solution with SMB or Copperas and; filter nitrate solution then recover the Ag with your preferred method.

Incinerate the solids including the metastannic acid; Then put the Incinerated solids in hot HCl; wash the solids a prepare boiling AR with a watch glass to leach Pt if it contains any.

After the recovery you can refine it or add it to your stock pot for later.


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## 9kuuby9

After stumbling upon this thread http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=51&t=9058 
I found out that upon addition of SMD in a Palladium nitrate solution it will participate a Complex Palladium salt; namely Na2Pd(SO3)2x2H2O. I guess you could try to participate metallic Palladium with copperas (in a Pd nitrate solution); maybe steve or freechemist has a input on this matter.


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## g_axelsson

I wonder what the solubility of that salt is? I got a voluminous precipitate and a yellow salt crystallizing on the surface... and the solution still have some palladium nitrate judging from the color.

This is what I got when adding SMB to an acidic palladium and silver nitrate solution.


And this is the day after, it's compacted a bit.


I think I'll go back to my old way, this made a bigger mess than dealing with silver chloride. I know I will learn some new tricks recovering from this mess. :mrgreen: 

What is the best way from here? Filtering off the precipitate and calcine it maybe?
I'll just treat the filtrate as before, creating silver chloride and get the silver from that, If there any values after that I'll just cement it with zinc.

Göran


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## 9kuuby9

I would say Keep adding SMB in small increments until no further participation.

filter the solution and rinse it with D.water; this salt is very insoluble and the water will only hold a very small amount of this salt. add the water you rinsed with to your stock pot. scavenge the remaining Pd with DMG from the primary nitrate solution.

after 3 hot D.water rinses with a gentle stir to insure proper washing of the salt.

freechemist's quote; "add excess aqueous ammonia, it dissolves giving a colorless solution, probably containing the complex cation [(NH3)4Pd]2+ and sulfite as anion. Boiling the salt in excess aqueous sulfuric acid - no halides, nor nitrates may be present! - it decomposes to metallic palladium, NaHSO4, SO2 and water."

Steve's qoute; "Dissolve the bright yellow Pd salt in excess ammonium hydroxide, filter and precipitate the canary yellow Pd ammonium chloride with HCl. This is the purified Pd salt we have made in the past. It gets converted to Pd metal via incineration or zinc in 5% HCl."

I have presented 2 alternative methods that have been covered in the past.

If all fails; calcine and refine it from their.

and then you can start recovering the silver in the first nitrate solution.

Has anyone used FeSO4 "Copperas" to participate Pd metal from a nitrate solution?; it normally should not form a complex salt; since their is no possibility for a double displacement.


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## 9kuuby9

upon the addition of FeSO4 to a Palladium nitrate solution; Palladium precipitates (edit) as a metal or as a sulfate salt (PdSO4) .


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## squarecoinman

9kuuby9 said:


> participated .



par·tic·i·pate (pär-ts-pt)
v. par·tic·i·pat·ed, par·tic·i·pat·ing, par·tic·i·pates
v.intr.
1. To take part in something: participated in the festivities.
2. To share in something: If only I could participate in your good fortune.
v.tr. Archaic
To partake of.
[Latin participre, participt-, from particeps, particip-, partaker : pars, part-, part; see part + capere, to take; see kap- in Indo-European roots.]
par·tici·pative adj.
par·tici·pator n.

:lol: 

scm


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## 9kuuby9

squarecoinman said:


> 9kuuby9 said:
> 
> 
> 
> participated .
> 
> 
> 
> 
> par·tic·i·pate (pär-ts-pt)
> v. par·tic·i·pat·ed, par·tic·i·pat·ing, par·tic·i·pates
> v.intr.
> 1. To take part in something: participated in the festivities.
> 2. To share in something: If only I could participate in your good fortune.
> v.tr. Archaic
> To partake of.
> [Latin participre, participt-, from particeps, particip-, partaker : pars, part-, part; see part + capere, to take; see kap- in Indo-European roots.]
> par·tici·pative adj.
> par·tici·pator n.
> 
> :lol:
> 
> scm
Click to expand...


oh I made a catastrophic error! :mrgreen:


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## g_axelsson

If you precipitate something it isn't participating any longer. :lol: 

I had to go on a business trip for a couple of days so the yellow palladium salt was left standing. During the week it compacted even more, forming a cake at the bottom and the yellow complex salt also made a crust on the inside of my beaker. The cake at the bottom seems to break down to a dark brown mud that doesn't dissolve in water but easily filters off. The crust I broke down with a glass rod and collected in the bottom of the beaker with the help of a spray bottle. Storing that for later processing.
To the rest of the now clear yellow solution containing silver nitrate and dissolved palladium salt I added zinc, taking everything back to metal and then I will wash it and dissolve it again in nitric and treat it as the first batch.

For future reference I add a link to the post where Freechemist gives a way to get palladium from the complex salt.
http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=51&t=9058#p87626
I will try that when I have a possibility to boil sulfuric acid.

I wish I had done some more research before doing this procedure, then I could have avoided this mess. I feel just like a noob right now. :mrgreen: 
... I'm taking the scenic route to palladium.

Göran


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## 9kuuby9

Good observation Göran; "Good judgment comes from experience, and a lot of that comes from bad judgment."

I will try to use Copperas to precipitate Pd from a nitrate solution and see how it goes


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## Marcel

It all sounds a bit complicated to me.
As it has been said, finechrush the material first, then your results will be better. I use a large hammer and a steel pot for that.
Add HCL to remove BMs.
From there dissolve either with HCl+Cl or HAP (hot AP).
Drop Pd with copper.
Treat the remaining solids with nitric. Let it soak for a long time (f.i. 1week), because the fine powder needs very long to fully dissolve the PMs.


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## 9kuuby9

well I use a iron pestle and mortar; but frankly it's really slow.

I can imagine if you work with a steel pot and a hammer that a lot off MLLC's start flying around when you are crushing them. and also use a breathing mask while doing so; because they release a very fine dust.

Maybe some has found a more efficient way of crushing MLCC's?


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## solar_plasma

I thought of a cheap little kitchen grinder for 10€ from Kloppenburg. Anyone who knows how long this will be durable to the hard ceramics? I think someone of you talked about that, was it you, Marcel?


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## 9kuuby9

solar_plasma said:


> I thought of a cheap little kitchen grinder for 10€ from Kloppenburg. Anyone who knows how long this will be durable to the hard ceramics? I think someone of you talked about that, was it you, Marcel?



maybe 15min. of continuous grinding? ; they are made from ceramics and Zirconium dioxide so thin metal blades wear off pretty fast...

Something like this would normally work fine;http://www.benl.ebay.be/itm/110998457104?ssPageName=STRK:MESINDXX:IT&_trksid=p3984.m1436.l2649

I don't know if they sell them in Germany? but these are made by a hobbys't in the US; so normally they are not sold.

Some pieces of iron or SS and a welder would accomplish it.


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## etack

solar_plasma said:


> I thought of a cheap little kitchen grinder for 10€ from Kloppenburg. Anyone who knows how long this will be durable to the hard ceramics? I think someone of you talked about that, was it you, Marcel?



I've tried to use a blender from the thrift store lasted about 200g then the blades were worn down. mortar is really hard too. I think a hammer mill or ball mill would work the best.

Eric


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## patnor1011

This never failed me. (your hands can but recovery is fast)


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## solar_plasma

If I don't figure out to build myself a ball mill, this one will be my favourite.


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## 9kuuby9

Very interesting! We need to improvise quite a lot on this subject ^^

I'll just go to my cellar and see what I can improvise and make with my metal scraps.


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## Marcel

Yawn Patrick, that´s an old hat. My grandmother used to grind them MLCCs like that ages ago...


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## solar_plasma

A family photo?


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## necromancer

great thread,

any updates to this (these) method (s)


look at that, looks like my lawyer wrote it :shock:


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## g_axelsson

Not any big revelations yet from me. The second time I tried to process MLCC:s it worked a whole lot different than the first time and I ended up with just a big mess of what I suspect a mixture of silver chloride with metastannic acid. I'll probably get on with experimenting with MLCC:s again in a month or two.

So far I got 14 grams of black powder in a small beaker, all recovered with zinc and nothing refined yet.

I read some time ago that going from a nitric solution with silver and palladium needs special treatment when adding chloride so you don't end up with a palladium - silver complex that is hard to break up but I haven't been able to locate it again. This forum is getting so big that even the oldtimers have a hard time to find what they are seeking.

Göran


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## joubjonn

What would you do with it? Send it to someone like Lou? 

I have about 700 grams of MLCC's and in the next month or two I do plan on going after the palladium but know I cannot melt it with the torch I have and I enjoy hoarding my gold but I'm at a loss on what to do with the palladium. Don't have enough to send to a refiner (who would probably rip me off anyway) and figured No one else who buys it near me would take black unknown powder. Maybe I can find someone around here to melt it for me. But I don't think I want to hoard it like my gold.


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## solar_plasma

All day long I think, search and read about NaOH with some H2O2 to dissolve tin and lead, I read stannates/plumbates/hydroxides back and forth, up and down, but neither I can find anything about using this method to prepare mlcc's, nor any reason, why this not should be a valid method. Has anybody else ever seen posts about NaOH on mlcc's?

I go on thinking and searching. I have 400g, now, and surely 100g left on a bunch of boards waiting to get scrapped for the last values.

By the way, today I found a strange flipchip (!), with goldplating beneath the silicon die. No bondwires ofcourse, but a lot plating. Strange...

Have a nice day all of you!


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## g_axelsson

I'm just hoarding until I have enough to do a proper refining.
When I have pure (relatively) I'll try to melt it together and then I can hoard the metals.

:mrgreen: 

I have no need of selling the metals and if I would I have a lot of other stuff to sell before I have to part with any metals I've dug out of old electronics. It would be another thing if I had bought the scrap in the first place.
It would be good to have a list of places that would buy precious metals in Europe, I have a better grip of the north American market than where I live.  

Göran


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## necromancer

silver chloride with metastannic acid mess (bla :evil

i am going nuts with these darn mlcc's

my post:
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=20518&p=211572#p211572


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## solar_plasma

Check out those two adding the search item NaOH. I believe you could smack two flies at once, metastannic gets soluble and AgCl will become Ag2O. Check for side effects first. Don't use KOH. Try with a small probe first, if you decide to try. Wait, if anyone wants to comment this.


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## necromancer

i have read every post i can find, i am just so confused. (noob attack)

my powder is still as it was. i am not jumping till i understand well

so......

my powder contains: (i think & hope)

silver, palladium, tin & maybe some other metals (cobalt, titanium)

*if i use the NaOH process & filter what will be left in the filter ? what will be left in the filtered liquid ?

what mixture of NaOH (Lye) & water do i use*

when i read about 30g of palladium from 1kg of mlcc it excites me very much & would love to learn this process
i have & get a good amount of mlcc to keep me busy

thank you for all your help


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## solar_plasma

Some PM salts must not be treated with NaOH (danger!). What I wrote would only be an idea, if those where in elemental form. I think it is best to wait. This seems to be more complicated than it looks like.


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## necromancer

yes it is, Lions, Tigers & Bears Oh My :lol: 

but i have went over my original math, it seems that i didn't use enough HCL

but they did soak for a month. should i restart from the "soak in HCL" to see if i missed any base metals ?
like dreaded tin. it did take forever to filter originally.


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## solar_plasma

Now I am confused. Didn't you add nitric, yet? If you did not add nitric, everything should be good. Only not enough HCl like you are assuming. But try with a small amount first.


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## necromancer

no nitric used, i was told to go with Lye or thiosulfate or Ammonium hydroxide, or set up a silver cell
confused i then started reading, got lost & am now still stuck at step 5.

i am at the same point as i was in this post:
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=20518&p=211572#p210365


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## solar_plasma

Forget the silver, leach the base metals, then get the palladium. The silver chloride will stay in the solids and can be recovered after you got the palladium...save it till when you feel bored. my two cents...

Until now, none of the different wet methods on mlcc's look perfect to me, just like cats.


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## necromancer

ok, thats what i was confused about. some say silver first, some say palladium first, will chase the palladium asap
will update in my post

thanks solar_plasma


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## solar_plasma

I know exactly what you mean, I was confused, too, when I read all the different styles. But in the end 30g Pd are maybe 500$, 100g Ag are 40$...almost trash. Trash that is nice to play with, when there is nothing else to do.

Just remember, there will be some traces of Pd in the AgCl and there will be some traces of AgCl dissolved in strong AR, if you choose to use the hard stuff for the last leaches.


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## joubjonn

Hey Necro, 

Can you post your method when you finish? I would be interested since I have about a kg of MLCC's myself I would like to process. What's your plan with the Pd once you get it?


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## necromancer

i have chose to take Goran's advice

it can be found in my mlcc post. i think the link is above


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## necromancer

nevermind, this "*is*" Goran's post


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## necromancer

joubjonn said:


> Hey Necro,
> 
> Can you post your method when you finish? I would be interested since I have about a kg of MLCC's myself I would like to process. What's your plan with the Pd once you get it?



Pd will be dried & stored, i dont have a good torch. unless someone close by wants to melt it for me ??? (Hint Hint)


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## g_axelsson

necromancer said:


> nevermind, this "*is*" Goran's post


No, it's Noxx forum... and I have followed your posts with great interest. 8) 

I'm sitting with a mess on my own that I created last summer. It looked good but I didn't let it sit in HCl as long as the first batch and when I added NaCl to it it turned into a thick mud with an unknown content. It probably is a mix of tin, palladium, lead, silver and copper in various oxidation stages and complexes with chloride and nitrate.
I tried to add a copper rod to cement palladium (the silver is in silver chloride form) and it somewhat worked, I got a palladium mirror on the surface and some branching palladium crystals on the rod after a couple of months. The mud changed color to white close to the rod (palladium chloride and nitrate cementing, depleting the mud), but the thick mud hindered circulation of the liquid so it was less than successful. The mud also locked in a lot of the cemented palladium metal particles.

Next idea I got was to treat it with NaOH to turn the silver chloride into silver oxide... and that is the stage it's in today. When I go on vacation I'm going to pick this experiment up and see what I can do to separate the metals. I also have another batch of MLCC:s that I'm going to process this summer. I guess I'm going to try the AR first to extract palladium and treat the left overs for the silver content.

As you see, it might be foolish to follow my advice on MLCC:s at this time... do it at your own peril! :mrgreen: 

Göran


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## bgp_scrap

I could be wrong here, 
But doesn't hokes say to use ammonium chloride for pgm's? 
I understand the cl would conflict with ag in solution.
But it would be alot easier then using zinc to cement 

Recently started collecying these, going back over 400 lbs (yes, 400) to scrape these small gems off.
I'll try a batch with smb and post my results and yeilds as well.


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## g_axelsson

bgp_scrap said:


> I could be wrong here,
> But doesn't hokes say to use ammonium chloride for pgm's?
> I understand the cl would conflict with ag in solution.
> But it would be alot easier then using zinc to cement





Hoke : Page 108 said:


> If your palladium is pure, and if your standard solution was prepared
> as directed, nothing will happen. This experiment shows
> that palladium differs from platinum in that it is not precipitated
> with ammonium chloride from an aqua regia solution from which
> excess nitric acid has been boiled off.
> Warm the mixture gently, and add a single crystal of sodium
> chlorate. Or, dissolve a pennyweight of chlorate in a little warm
> water, and add a drop at a time. There will be considerable fizzing,
> and as it subsides, add another small crystal or another drop. The
> solution should be just short of boiling. After the addition of a little
> more of the chlorate, a change in color will be noted. Stir the
> mixture with a glass stirring rod; soon a dark red precipitate will be
> seen, floating on the surface and then sinking. Continue to add
> chlorate, a little at a time until the liquid is almost colorless, and
> then let cool. This red powder is palladium ammonium chloride chemically
> much like the orange powder above.



To me it was easier to use zinc to get all PGM:s in one go and collect the black powder until I have enough to warrant a separation and refining of the different metals. Even though the MLCC:s probably contained mostly palladium it was easier to add it together with other batches with other PGM:s. Some time in the future I'll refine it.

Göran


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## Rocky888

Goran, I have used your method twice, once with surface mount resistors and once with MLCC's. I have achieved good results ending up with a palladium nitrate solution. The only thing I did different was that I heated the HCL after soaking in room temperature HCL for two weeks. As soon as I heated it the reaction started again. I think it would be very hard to gage when all base metals have been removed without heating. Can hot HCL dissolve some palladium ? I thought HCL could only dissolve palladium if it is finely divided.


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## Harold_V

Rocky888 said:


> Can hot HCL dissolve some palladium ? I thought HCL could only dissolve palladium if it is finely divided.


It will readily dissolve oxidized palladium.

Harold


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## lunker

Harold,

Could the mlcc s first be boiled in hcl to remove tin and lead. Then crushed and roasted to convert the palladium to a oxide? Then you could leach the pd out and go after the silver with nitric once you expelled the free hcl? Or would the palladium require to high a tempeture to oxidize?

Regards


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## Harold_V

lunker said:


> Harold,
> 
> Could the mlcc s first be boiled in hcl to remove tin and lead. Then crushed and roasted to convert the palladium to a oxide? Then you could leach the pd out and go after the silver with nitric once you expelled the free hcl? Or would the palladium require to high a tempeture to oxidize?
> 
> Regards


I'm probably the wrong person to ask, although it would be my opinion that what you proposed wouldn't work well. If the palladium was sponge, with a lot of surface area, yeah, it might work, but solid pieces would experience only surface oxidation, so the process wouldn't really solve the issue. 

Harold


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## lunker

Really never any short cuts when it comes to refining. Thought the 2 percent pd range might make it plausable.
Thanks for responding


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## Erceg

So un-oxidized palladium will not be dissolved in hot HCl but will dissolve in very dilute AP (HCl + air bubbler)?
How much does palladium oxidase in H2O (from dilute acids)? I suppose it should not be much?


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## patnor1011

I believe that Pd is in form of paste sandwiched in a layers in them so it may be dissolved easier than if it would be like solid pellet or something like that.


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## Erceg

Yes, it is, but i don't want it to dissolve. I'm depopulating RAM in HCl with air bubbler and i want MLCC to just fall of with chips so i don't need to extract small amount of Pd from large volume of solution rather accumulate them for future separate extraction of Pd.
If that is not possible I'm planning to do as Geo suggested with addition of grinding MLCC with gold flakes, then dissolve Pd in nitric, wash, filter, dissolve gold in AR or HCl/Cl....
Then I'll have concentrated solution of Pd and Au and poor solution of Pd with base metals. From that poor solution Pd would be extracted with Zn or just left for stock pot till I learn how to deal with it before disposal?


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## etack

I think you are over thinking the amount of Pd in there. What you will have is a small amount of Pd mixed with gold and it will be a pain to remove. You are talking about a minuscule amount of Pd for this much work. You would be better served to remove the MLCCs before you put them in the AP. 

Eric


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## Erceg

I know it would be better but there is about 4lbs of memory so it would be a While to remove MLCC with flat screwdriver. More because i plan to process much more than 4lbs in the future so i must find faster method. Yes it is a small amount of Pd but it must be removed because of gold purity and when I already need to remove it I can try to collect it


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## patnor1011

Use heat gun, it takes about 15 seconds to heat stick and bang everything off. Much faster and efficient than using buckets of HCl.


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## Rocky888

If I understand this correctly, palladium will not dissolve in hot HCL unless it is finely divided or oxidized and it won't oxidize until it hits 800 degrees celcius. So what is palladium paste made from? Is it made from oxidized or finely divided palladium? When I processed some MLCC's I tested my base metal leach HCL with DMG and didn't find any palladium, but is that even a valid test when lots of base metals are present? Just wondering if I am losing any palladium before I process a larger batch. Any answers to my questions would be greatly appreciated.


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## Erceg

Patnor, how hot can your heat gun get. Mine goes to about 520 C and it takes more like 25s for one side and few more for other side of ram stick.


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## patnor1011

Have no clue but I was using cheap lidl one and it was not good enough so then I bought more expensive one from hardware store and it is much better. I hold them really close and all it take is few seconds to solder soften, then nice bang on side of bucket and things are flying off. I was using hotplate and sand too and it was fast too, I started to lay them inside pan and by the time I lay last one first was teary to go, so I was constantly removing and putting them in and out.


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## Erceg

Thank you very much for your advice. I appreciate it very much. I taught about sand bath. Would something like this be enough to heat it up or do I require a torch?
http://www.coolinarika.com/repository/images/_variations/c/7/c76140722593aaa1400ee19e7e990518_view_l.jpg


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## necromancer

g_axelsson said:


> necromancer said:
> 
> 
> 
> nevermind, this "*is*" Goran's post
> 
> 
> 
> No, it's Noxx forum... and I have followed your posts with great interest. 8)
> 
> I'm sitting with a mess on my own that I created last summer. It looked good but I didn't let it sit in HCl as long as the first batch and when I added NaCl to it it turned into a thick mud with an unknown content. It probably is a mix of tin, palladium, lead, silver and copper in various oxidation stages and complexes with chloride and nitrate.
> I tried to add a copper rod to cement palladium (the silver is in silver chloride form) and it somewhat worked, I got a palladium mirror on the surface and some branching palladium crystals on the rod after a couple of months. The mud changed color to white close to the rod (palladium chloride and nitrate cementing, depleting the mud), but the thick mud hindered circulation of the liquid so it was less than successful. The mud also locked in a lot of the cemented palladium metal particles.
> 
> Next idea I got was to treat it with NaOH to turn the silver chloride into silver oxide... and that is the stage it's in today. When I go on vacation I'm going to pick this experiment up and see what I can do to separate the metals. I also have another batch of MLCC:s that I'm going to process this summer. I guess I'm going to try the AR first to extract palladium and treat the left overs for the silver content.
> 
> As you see, it might be foolish to follow my advice on MLCC:s at this time... do it at your own peril! :mrgreen:
> 
> Göran
Click to expand...


not foolish at all, by following your thread i have a very small test tube with cemented palladium
you may not think your doing the right thing but i am new to palladium recovery & your post has been super helpful (Thank You)

since making a huge mess of the first 3 lbs of MLCC's i now have 4.5 lbs more to make less of a mess of 8)


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## g_axelsson

necromancer said:


> not foolish at all, by following your thread i have a very small test tube with cemented palladium
> you may not think your doing the right thing but i am new to palladium recovery & your post has been super helpful (Thank You)
> 
> since making a huge mess of the first 3 lbs of MLCC's i now have 4.5 lbs more to make less of a mess of 8)


Great! That brings a big smile to me. 8) 

I'm still no further on my mess. I have dried the mud up and is going to incinerate it and continuing from that point when I get some time.

Göran


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## patnor1011

Erceg said:


> Thank you very much for your advice. I appreciate it very much. I taught about sand bath. Would something like this be enough to heat it up or do I require a torch?
> http://www.coolinarika.com/repository/images/_variations/c/7/c76140722593aaa1400ee19e7e990518_view_l.jpg



Sure, put a shallow round or square cake pan on top, fill with about 2cm of sand and you are good to go. I do not put much sand there as the more you put in the longer it take to heat and work. I use stainless steel forceps the type one use when fishing, you will need to collect IC which fall off if material stay long in hot sand.


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## Erceg

That is the plan, with fire brick around to keep heat. 
Than you. Great thread overall.


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## kjavanb123

Smelted a batch of 2lbs of mixed SMD capacitors, resistors, and tantalum capacitors using 2 parts borax, 1part cryolite, melted the, in an induction furnace, twice, second time without cryloite.




This is after first melt poured into a mold,



Put slags and metals back to furnace this time with more borax and no cryolite,



The metals are in dilute nitric acid, I am expecting ruthenium oxide, and tantalum in the mix which are soluble in nitric acid.

Best regards,
Kevin


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## Lou

Ta is not soluble in any acid but HF and mixtures containing it.


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## kjavanb123

Lou,

My bad, I meant Ta and Ru are not soluble in nitric or any organic acids. So these metals are dissolving in nitric acid so will have to check on them on weekends.

Regards
Kj


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## Anonymous

Just a quick one, why are you expecting those metals in particular ?


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## necromancer

thanks Kevin, i always enjoy your posts


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## kjavanb123

spaceships said:


> Just a quick one, why are you expecting those metals in particular ?



I had a lot of Ta caps and RuO resistors in the mix of my materials along with SMD capacitors.


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## kjavanb123

necromancer said:


> thanks Kevin, i always enjoy your posts



Thanks necromancer, since ai got the induction furnace I have been trying to do the projects I had in mind, I will do a project smelting catalytic converters using this furnace and will post the result soon.

For those of you following my shaker table project, the discharged materials finally got to the lab and expecting their results soon.

Best regards,
Kevin


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## Platdigger

So Kevin, how do you propose to use induction, with a heel? 
I mean how will you get the cat material to melt?


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## kjavanb123

Platdigger,

There was a detail post here talking about just that, I can't find it yet, but my first step would be pulverize cats to fine mesh, find the right flux, ball mill flux, any collector metal and pulverized cats to get them mix.
Then melt in a small crucible.

Regards
Kevin


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## wicky

necromancer said:


> silver chloride with metastannic acid mess (bla :evil
> 
> i am going nuts with these darn mlcc's
> :
> my post:
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=20518&p=211572#p211572



Hey necromancer,

What is metastannic acid and how dose it forms in mlcc's. Tin nitrate or Tin oxide?


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## g_axelsson

wicky said:


> Hey necromancer,
> 
> What is metastannic acid and how dose it forms in mlcc's. Tin nitrate or Tin oxide?


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

/Göran


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## MrMylar

9kuuby9 said:


> I'm glad to help you out. I know that participating gold with SMB or Coperras in a chloride solution causes PGM's drag down. In a nitrate solution it can fully participate Pd.
> 
> The best way of recovery is to use eficient methods in recovering vairous metals;
> 
> U can crush the MLCC's wich is time consuming but it will leach faster and have better yield results.
> 
> I first tend to use nitric 50/50 D. water to leach the base metals including Ag & Pd; after 2 or 3 leaches of fresh nitric solution; filter the solids out including the metastannic acid.
> 
> Drop out the Pd in the filtered nitrate solution with SMB or Coperras and; filter nitrate solution then recover the Ag with your preferred method.
> 
> Incinerate the solids including the metastannic acid; Then put the Incinerated solids in hot HCl; wash the solids a prepare boiling AR with a watchglass to leach Pt if it contains any.
> 
> After the recovery you can refine it or add it to your stock pot for later.


Since this is my first time dealing with MLCC's and have read so much on processing these, I have accumulated a few lbs worth of them so far. And since I'm going to start my first batch today sometime (hopefully) and go for it, this method seem to me, to be the quickest way to refine and recover these MLCC's.

I have been reading and waiting for about 3 years now, and now is my time to process these. I've seen some videos that now that I understand it better, some of those videos and other information is doing 10 things when you could have just done 4 things and achieve the same result(s).

Since I never refined for palladium before, this is something I can understand more so now, just by rereading threads and other information. I am confident that the method quoted above is something I'm definitely going to implement. It makes much sense to me. I have been holding and collecting these mlcc's for years now, and now that I've done my fair share of refining gold and silver bearing items. Now I'm ready for the Palladium. It's less than gold and it's more than silver.

I am thinking that these are easier to refine than one may think. 

Let me ask something.

*a)* Would Muriatic acid work for this or straight HCL? My Muriatic Acid is 31.45% HCL
b) Will MAPP gas (disposable tank) be hot enough to melt the palladium? I read 3600F+ with air, and 5800F with oxygen is how hot MAPP gas will get. The one with air, a person would have to introduce air into the torch somehow? And does this mean getting a acetylene torch?

I just remembered that I need to get some Nitric acid. Using the Nitric acid, have anyone calculated how much (approximately) nitric acid is needed to dissolve all it can with 1lb. of the mlcc's. From looking at my own, 1 lb of them can easily fit in a 2000mL beaker with plenty of space left. 

According to this method, just to get to the palladium, it already saved time and steps to take. When I think about it, from what I've learned over the years refining, every method I've read and saw all have you understanding that it's going to take days to do it when you can actually get to see some palladium that same day. From powder to metal. I am glad I reread many threads here on the forum.

This method eliminates the need of adding zinc to it and other steps I've seen before. 

As I wait on some more acid, I'll just crush them up and have them ready for solution. Once I get it going, I'll post my results here. 


Thanks.


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## Lou

Doing them wet is ill advised. 

ferrous sulfate is more than a little bit inefficient at precipitating palladium from nitrate. 

MAPP won't melt Pd as is.



Have you been reading *here* for 3 years now? I suspect you have.


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## Anonymous

Are Palladium salts quite toxic?


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## Lou

Not particularly, especially so when compared against gold, which is quite cytotoxic. 

As a general rule, treat everything as if it could kill you and be sure to exercise good care to prevent cross contamination, particularly with platinum. 

Our practice is to have a container with a swivel lid and a trash bag liner labeled "burnables" for gloves, wipes that may have contacted precious metals.


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## MrMylar

Lou said:


> Doing them wet is ill advised.
> 
> ferrous sulfate is more than a little bit inefficient at precipitating palladium from nitrate.


Can you elaborate more on this?


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## Lou

Smelt them.


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## kurtak

Lou is correct - smelting is the way to go :!: 

Its discussed in detail here :arrow: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=20710&hilit=cryolite#p212704

You need a good gas furnace & silicon carbide crucibles & a cone mold - do not try it in an electric furnace with graphite crucibles - the flux will destroy the elements in an electric furnace & graphite crucibles will not hold up to the flux ether.

It is next to impossible to wash/filter all the leach out of the ceramic using a wet/leach process even with a vacuum filter set up - the ceramic gets broken down into an ultra fine powder in the leaching process - so fine that it acts like the clay used to seal the bottoms of ponds - in short leaching makes a BIG mess

Also - I hope you are aware that not all MLCCs are made with Ag/Pd some (many/most) are made with Ni/Cu - use a magnet to remove those from the Ag/Pd ones 

Kurt


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## johnny309

Also - I hope you are aware that not all MLCCs are made with Ag/Pd some (many/most) are made with Ni/Cu - use a magnet to remove those from the Ag/Pd ones 

Kurt[/quote]


The ones removed with a magnet still contain a little silver or Ag/Pd to the soldering pads( terminals of the capacitor).The inner layers are BME(base metals...Ni,Cu,etc). 
So ,those ones can be processed with the chip resistors,which have the same Ag/Pg substrate at the soldering pads.
Reference can be found in the producers datasheet,company like VISHAY or DALE.


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