# Refining MLCC´s for Palladium and Silver !



## Lars100

All,
I managed to get together quite a pile of MLCC's which are of 2005 or older... Im far from a chemist but have been working with electronics for many years. Got on the track with Palladium when I learned about all the cathalyst´s being stolen from cars and realized that I had these MLCC´s.
So my goal is to extract as much Palladium and Silver as I can.
Started watching videos on YouTube how to do this refining and brought together necessary acids (so far...). Placed the MLCC´s in pet bottles with about 15% HCL to get rid of the tin (and perhaps outside nickel). Believe I was pretty succesful as I ended up (after about a week) with a purple transparent liquor with grey mass in the bottom (tin ?).
Out with the MLCC's and let them just dry up for a while. Put the purple liquid aside.
Bought two mixers with extra blades and grinded the MLCC's to dust (almost). Then into new pet bottles and added concentrated Nitric acid. Red smoke and red fluid. The mass changed color into greenish/grey.
Let it stand for about a week (shaking every day). Out of the bottles and filtered. I have saved the grey green mass in the filters (dont want to throw away...yet).
The components (whats left of them) into a plastic tray for keeping.
The filtered fluid is black/green and fairly transparent.
Added concentrated HCL and the fluid changed color to dark red and in the bottom a separated beige/red mass appeared (silver ?).
I believe this is correct so far...
I have taken some other measures from here but it doesnt seem right.
For ex. adding sodium and formic acid to the dark red fluid...and heat to about 80C. If I filter that potion and heat again it will only become a black mass.
If I pore Nitric Acid in that black mass then it melts into a orange/brown tranparent fluid (which in a way must be right but only takes me backwards...) !
Im a bit stuck...


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## orvi

Red-orange-brown colour is relatively what you are looking for. If you are in doubt, cement it out  redissolve everything and cement on copper. Anything of value will come out of solution, but you need air bubbler or magnetic stirrer/mechanical stirrer. Liquid must be agitated while precipitating PGMs on copper.


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## Yggdrasil

I believe you have your chemistry wrong. Silver will transform into SilverChloride when it finds any chlorine ion. It do not dissolve in acids. It is a white fluffy substance that take time to settle. The substance you have is probably a mix of ceramics and metastannic acid. It is a nightmare to filter so most of us hate it. Dissolved Pd salts with chlorine will usually be brownish red, not bright red.
Did you do a stannous test?


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## Yggdrasil

orvi said:


> Red-orange-brown colour is relatively what you are looking for. If you are in doubt, cement it out  redissolve everything and cement on copper. Anything of value will come out of solution, but you need air bubbler or magnetic stirrer/mechanical stirrer. Liquid must be agitated while precipitating PGMs on copper.


You beat me to it again
I will need to move faster


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## Lars100

Im not sure I know what You talk about... Cement it out ? How do I do that ? Cement on copper ? Do I just put a copper plate in the red-brown liquid and wait for the palladium to stick ?
- I will take some pictures and show You what I got so far.
Please have patience with me. I basically have no clue and no earlier experience...


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## Yggdrasil

Lars100 said:


> Im not sure I know what You talk about... Cement it out ? How do I do that ? Cement on copper ? Do I just put a copper plate in the red-brown liquid and wait for the palladium to stick ?
> - I will take some pictures and show You what I got so far.
> Please have patience with me. I basically have no clue and no earlier experience...


Another reason to take it easy.
The salts from PGMs are very toxic and can lead to severe health problems and death.
Cementing means putting in a more reactive metals so they swap place. But with PGMs it is crucial that the liquid moves quite fast to dislodge the cemented metal so it do not pasify the copper. An air bubbler will fix that.


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## Lars100

Thanks ! Ime trying to protect with ventilation, fans, rubber gloves and protective glasses. I don touch anything with bare hands.
Ok, please see the attached pics. 
I look forward to hear Your comments /questions !


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## Yggdrasil

Silver chloride is bright white and fluffy. So the last picture may or may not be silver chloride, do not let it dry.
But you have to wash it clean first, until there is no color in the liquid. The liquid may contain some of your values.

Which lead to:
Did you ever test it with stannous?
Without a test it may be all trash, and you are wasting your acid.


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## Lars100

Thanks for input !
Ehh...Stannous-test...how do I perform such a test ?
Air-bubbler ? Any brand, type You can recommend ?


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## Lars100

And furthermore...clean the liquid ? How do I do that (and with what) without wasting all the goodies ?


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## manorman

Bare hands a handling toxic substances not a good idea. You need to slow down and read before you kill yourself or someone else.


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## orvi

MAN, PGM solutions and NO GLOVES ??? Seriously ?


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## Lars100

No no...See above...RUBBER GLOVES !!!


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## galenrog

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.


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## Lars100

Im glad I gave You something to talk about !
I am certainly aware of the danger with these products and keep myself protected (as much as I can).
The pictures from today (with bare hands) were just something I took with speed as I wanted to have something to show here.
We can of course continue to discuss safety or we can move forward and let me know what I need to do in order to purify the metals I got !
- P.S. Im not saying that I will live forever but I started out with this project in Nov-21 and it´s now April-22.
Im still feeling well despite the fact that I´ve had Covid twice.


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## Yggdrasil

Lars,
We recommend or more command, one thing from people coming here.
That is self study, read on the forum, 
there is a handy search function, the information can be a bit overwhelming in the beginning.

And it is a must to read C.M. Hokes book. She takes you through most of what you need to know. 
It is old so safety was not as today so I believe some chapters has been modified for that.

Some of the members has the link to the book in their posts.

It goes to the concept, give a man a fish and he eats today or learn him to fish and he is fed the rest of his life.

So please read, search and study. When you need help, ask questions about the issue at hand and you will be helped.


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## Yggdrasil

Lars100 said:


> Im glad I gave You something to talk about !
> I am certainly aware of the danger with these products and keep myself protected (as much as I can).
> The pictures from today (with bare hands) were just something I took with speed as I wanted to have something to show here.
> We can of course continue to discuss safety or we can move forward and let me know what I need to do in order to purify the metals I got !
> - P.S. Im not saying that I will live forever but I started out with this project in Nov-21 and it´s now April-22.
> Im still feeling well despite the fact that I´ve had Covid twice.


That is why we ask you to do a stannous test, it will show if you have values in there. 
And the way you ask what it is, clearly tell that you have not studied enough.

Stannous refers to StannousChloride which is Tin dissolved in HCl.

When that meets Gold, Pt or Pd in solution, it forms colloids with distinct colors. 
Purple for Au, Orange for Pt and greenish blueish color mix for Pd.

Search and you will find pictures of it.
Take your solution and drop one drop on some paper and then one drop of stannous on the same spot after.

If there are values you will see it immediately.

If not, the solution can be poured into the stock pot.


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## Yggdrasil

Lars100 said:


> Thanks for input !
> Ehh...Stannous-test...how do I perform such a test ?
> Air-bubbler ? Any brand, type You can recommend ?


Aquarium bubbler of any kind


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## Lars100

Many thanks Yggdrasil !
I appreciate that You point me in the right direction !
Have a nice Easter (and I guess I´ll be back here next week) !


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## Yggdrasil

Lars100 said:


> And furthermore...clean the liquid ? How do I do that (and with what) without wasting all the goodies ?


Since you do not say what you are referring to with clean the liquid, I presume it was referring to the SilverChloride. It is whiter than snow and what you show that may look like AgCl is dirty and has liquid with potential value in it. Fill it with distilled or DI water shake or stir it well, get it properly hot and then siphon off the liquid after it has settled.
Then do it again.
As long as the liquid test positive to stannous you keep it for further processing.
When it no longer test positive set it aside for stock pot and waste treatment.
What is left in the beaker should now be as white as fresh snow.
It can be set aside for later conversion, but do not let it dry or be subjected to light.


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## Lars100

Ok, got it ! I understand that decanter and/or siphon off are important ways to separate fluids in chemistry !


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## Yggdrasil

Lars100 said:


> Ok, got it ! I understand that decanter and/or siphon off are important ways to separate fluids in chemistry !


Is that what you got from my reply?
I suggest you read it again.


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## Lars100

Im not so sure why You sound "semi-angry" all the time or believe that You are talking with an idiot !?
My concern with "washing" material is to loose out of the good stuff if You do just "washing", Now You did explain to me how I should keep it all together and let it all remain until I have one jar with the silver and one bottle with nothing nice left. I understand what procedure You mean when You talk about "washing" (which is something I already been doing earlier in my process...but without calling it washing). Im sorry that Im not familiar with all of Your terms.
- I have learned a lot already with the conversation with You and I´m really really greatful. But Im not stupid !


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## Ohiogoldfever

Many members have been through hundreds of guys new to this hobby who don’t heed the warnings. Guys who don’t practice safety and who ask questions that prove they don’t really have a reasonable grasp of what they are trying to do. 

I’m sure if he’s coming off as frustrated it’s because you want the fast answers and are not willing to read into the things your asking about. 

Platinum group metals will poison you. You take photos of your holding filthy jars with bare hands yet claim your not stupid. I’m sure you are right but you are not doing a great job of representing yourself. 

If you wish for people to invest time into helping you then you’ll need to prove you’re willing to help yourself first.

Good luck. Stay safe.


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## Lars100

Now I´ve read a bit about the "Stannous-test" and it looks rather inconclusive to me...
Don´t get me wrong I´will perform it and have already ordered some 99.9% tin but there are some comments to be made. First the fluid itself can be made in many ways and with a variation of the tin percentage. Secondly the way to perform it and where to apply it varies quite a lot to -one says that You should drip the fluids on a paper.
And the result seems to be variation of colors. For ex. Palladium getting black instead of blue.
Anyway, I will perform this test in the beginning of next week and then we´ll see what comes out of it !


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## Ohiogoldfever

It’s one of the most important things to know before you proceed. 

I use 2 grams of Tin shot in 50ml of Hydrochloric. Filter after dissolving the tin. Works a treat.


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## Ohiogoldfever

The difference in testing style are purely preference. 

Use filter paper, or a testing dish, spoon..... All you’re doing is maintaining a controlled space for your sample.


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## gldfever87

Thank you all for the information for palladium and silver chloride. Knowing what test to run and steps to take make a huge difference. I have been doing gold for about six years, self thought and practice on small scale first .I've recently starting doing palladium, silver and gold and iridium. Very helpful thank you all...


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## Geo

This is for future information as I'm not sure I can help with what you have already done. 
Use a ferrite magnet to separate the magnetic and non-magnetic MLCC's. Lightly magnetic can be added to the non-magnetic ones. Strongly magnetic ones can be discarded. There is still a potential for silver but chasing it is not worth it. Take the money it would cost you to try and refine them and just buy silver. After magnetic separation, leach in 50/50 HCl and water to remove the solder. After this leach, decant the solution as waste. Rinse the material well. Roast the material to a low red heat. This sets the alumina ceramic and makes it harder to dissolve. Remove from heat and allow it to cool. Crush the material but don't mill to powder. Just crush. Leach the material in nitric acid. The least amount of volume as needed. Once the metal is dissolved, the nitric acid will start breaking down the alumina ceramics. All you want to dissolve is the metal. Decant the solution and leach the material again in nitric acid to ensure you got all the metal. Decant into the same container and filter well. Add HCl to drop silver as silver chloride. This will leave Pd in solution. Filter the AgCl from solution. The solution should be some color of red. This will give you the cleanest solution to work with. Precipitating the Pd with ammonium chloride + chlorine gas will give you a red salt of Pd or cement onto copper to obtain a slightly impure palladium metal in one go. 
Learn how to make and use stannous chloride.
PGM's (platinum group metals) in solution are both toxic and poisonous. Avoid contact with solution or aerosols or contaminated materials. Wear gloves and a respirator or at least a N95 dust mask to prevent breathing aerosols.


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## MicheleM

@Geo HCl +H2O2 could replace HNO3 to dissolve finely divided Pd, Do you agree?


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## Geo

MicheleM said:


> @Geo HCl +H2O2 could replace HNO3 to dissolve finely divided Pd, Do you agree?


Yes, but it should be 30% H2O2 and not the 3% you get at the pharmacy. Otherwise your just diluting the solution. Hair bleach from beauty supplies will also work.


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## Lars100

Geo said:


> This is for future information as I'm not sure I can help with what you have already done.
> Use a ferrite magnet to separate the magnetic and non-magnetic MLCC's. Lightly magnetic can be added to the non-magnetic ones. Strongly magnetic ones can be discarded. There is still a potential for silver but chasing it is not worth it. Take the money it would cost you to try and refine them and just buy silver. After magnetic separation, leach in 50/50 HCl and water to remove the solder. After this leach, decant the solution as waste. Rinse the material well. Roast the material to a low red heat. This sets the alumina ceramic and makes it harder to dissolve. Remove from heat and allow it to cool. Crush the material but don't mill to powder. Just crush. Leach the material in nitric acid. The least amount of volume as needed. Once the metal is dissolved, the nitric acid will start breaking down the alumina ceramics. All you want to dissolve is the metal. Decant the solution and leach the material again in nitric acid to ensure you got all the metal. Decant into the same container and filter well. Add HCl to drop silver as silver chloride. This will leave Pd in solution. Filter the AgCl from solution. The solution should be some color of red. This will give you the cleanest solution to work with. Precipitating the Pd with ammonium chloride + chlorine gas will give you a red salt of Pd or cement onto copper to obtain a slightly impure palladium metal in one go.
> Learn how to make and use stannous chloride.
> PGM's (platinum group metals) in solution are both toxic and poisonous. Avoid contact with solution or aerosols or contaminated materials. Wear gloves and a respirator or at least a N95 dust mask to prevent breathing aerosols.


Hello !
Soo many thanks !!!
I believe I got the hang of it and have made it quite succesfully to -"The sollution should be some color of red". That is exactly what I´m having ! And I tried to get rid of de silver just by decant/siphon it. But now... -"Precipitating the Pd with ammonium chloride + chlorine gas will give you a red salt of Pd" sounds very scary to me...(even me...) ! Chlorine gas ? How can I work with Chlorine gas ? Sounds better to -"cement onto copper to obtain a slightly impure palladium metal in one go". But how does it work (I have never done it) ? Do I just put sticks of copper into the fluid and wait for it to stick ? For how long ? How can i be sure to get it all ? And wont the copper disolve into the acid ?
Sorry for all my questions...but I think I got the red fluid right and I don´t want to spoil it all now...


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## kurtak

Lars100 said:


> Sounds better to -"cement onto copper to obtain a slightly impure palladium metal in one go". But how does it work (I have never done it) ? *Do I just put sticks of copper into the fluid* and wait for it to stick ? For how long ?


Per the bold print (in above quote) - *NO *

Read *BOTH* of these threads & read them *COMPLETELY*









When In Doubt, Cement It Out


When In Doubt, Cement It Out This is advice I often give to new members who find they've created a bit of a mess, and they're wondering how to recover their values (gold, silver, PGMs, etc.). Perhaps they've followed a process they've seen on YouTube that left out some important details...




goldrefiningforum.com













Fuzz Button Interconnects, need some advice


okay, back a while ago, I found a bunch of fuzz button interconnects... like the ones from this thread: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=34&t=16018&hilit=fuzz+button&start=20 after doing some research on them, I was figuring on Be/Cu/Au wire was most likely what I was dealing...




goldrefiningforum.com







Lars100 said:


> How can i be sure to get it all


Testing with stannous chloride - as well - when you are working with Pd you should have DMG on hand for doing conformation testing 

Kurt


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## Lars100

kurtak said:


> Per the bold print (in above quote) - *NO *
> 
> Read *BOTH* of these threads & read them *COMPLETELY*
> 
> 
> 
> 
> 
> 
> 
> 
> 
> When In Doubt, Cement It Out
> 
> 
> When In Doubt, Cement It Out This is advice I often give to new members who find they've created a bit of a mess, and they're wondering how to recover their values (gold, silver, PGMs, etc.). Perhaps they've followed a process they've seen on YouTube that left out some important details...
> 
> 
> 
> 
> goldrefiningforum.com
> 
> 
> 
> 
> 
> 
> 
> 
> 
> 
> 
> 
> 
> Fuzz Button Interconnects, need some advice
> 
> 
> okay, back a while ago, I found a bunch of fuzz button interconnects... like the ones from this thread: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=34&t=16018&hilit=fuzz+button&start=20 after doing some research on them, I was figuring on Be/Cu/Au wire was most likely what I was dealing...
> 
> 
> 
> 
> goldrefiningforum.com
> 
> 
> 
> 
> 
> 
> Testing with stannous chloride - as well - when you are working with Pd you should have DMG on hand for doing conformation testing
> 
> Kurt


Hi Kurt !
Many thanks for the threads ! 
Actually in the first thread they are saying that You can basically just put copper sticks in the fluid...but that it doesn´t work well... 
- I can make such a "blower" with my 3D-printer. Great...but not great  It seems like whatever I do here will end up in contaminated PD...
So...I will back off a little bit and do the stannous test (just waiting for my tin) and then maybe also test with DMG.
I will let You know of the outcome of these tests and then, hopefully, proceed to have all my liquid ready at that level.
From there I will test various methods to get pure PD out of it (if it is even possible). 
When started out I had roughly 30kg of MLCC´s so You can understand that it´s keeping me a bit busy (and worried that it will all just be rubbish)...


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## kurtak

Lars100 said:


> Actually in the first thread they are saying that You can basically just put copper sticks in the fluid.


With gold & silver that is for the most part true - cementing PGMs is a bit different then cementing gold/silver - with PGMs you NEED to have an aggressive agitation of the solution 

Please re-read the threads - read them until you FULLY understand - it's important that you understand this & I don't have time to re-post (here) what is already posted in those threads - which is why I gave you the links to the threads

Kurt


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## Lars100

kurtak said:


> With gold & silver that is for the most part true - cementing PGMs is a bit different then cementing gold/silver - with PGMs you NEED to have an aggressive agitation of the solution
> 
> Please re-read the threads - read them until you FULLY understand - it's important that you understand this & I don't have time to re-post (here) what is already posted in those threads - which is why I gave you the links to the threads
> 
> Kurt


Hi Kurt !
Many thanks for your thoughts but
I suggest you read my reply too !
I'm not going in there before I have a solid solution.
I hope to land this airplane and in the end maybe...just maybe...I have some good ideas to share too !


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## MicheleM

OT for @Geo :do you know this YT channel? your video inside : https://m.youtube.com/user/propeter13


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## orvi

Until you start to work with large batches, you need to obtain skills and understand the safety measures. This isn´t a healthy journey 
Working in 1 L beaker and filtering the 1 L of the solution isn´t big deal, but working in 20 L reactor or worse - 5 gallon bucket isn´t the same thing. Everything get more laborius, more dangerous and possibility of accidental spillage or leak is much bigger. Long gloves are a must, and I strongly recommend a fume hood.
You need to work out how to heat big volumes of liquid safely. This is the tough part. 
Once you have it all cleared up, you need to build a cementing vessel with good aquarium pump to stirr the solution in close proximity to the copper bar. I will say that for the first time, you should avoid NH4Cl+Cl2 palladium precipitation. Building a cementation vessel is much easier and you will end up with little material in the end, which will be much easier to refine.

Chemistry is unforgiving, and that´s why it is wise to train first and then make it happen. You need to learn how to use stannous chloride test - without stannous chloride, you will be partly blind - you won´t know what is in the juice. Obtain a small sample of Pd, or process some of the MLCCs as Geo instructed you. You will have Pd solution in hand and you can then test and observe what it should look like.

Also, kurtak gave the thread on proper PGM cementation. It is necessary to understand why all these things are done as they are. Many things in refining can go wrong, much more often than one can imagine. And you will need to know how to deal with such situations.


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## Geo

MicheleM said:


> OT for @Geo :do you know this YT channel? your video inside : https://m.youtube.com/user/propeter13


I do not.


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## Geo

Lars100 said:


> Hello !
> Soo many thanks !!!
> I believe I got the hang of it and have made it quite succesfully to -"The sollution should be some color of red". That is exactly what I´m having ! And I tried to get rid of de silver just by decant/siphon it. But now... -"Precipitating the Pd with ammonium chloride + chlorine gas will give you a red salt of Pd" sounds very scary to me...(even me...) ! Chlorine gas ? How can I work with Chlorine gas ? Sounds better to -"cement onto copper to obtain a slightly impure palladium metal in one go". But how does it work (I have never done it) ? Do I just put sticks of copper into the fluid and wait for it to stick ? For how long ? How can i be sure to get it all ? And wont the copper disolve into the acid ?
> Sorry for all my questions...but I think I got the red fluid right and I don´t want to spoil it all now...


I use copper when copper is already in the solution. The "go to" when cementing PGM's is normally zinc powder or turnings. Add small amounts incrementally as the reaction is exothermic and can get out of hand quickly. The reaction is complete when the solution loses all color except maybe a light green tint that will not cement out, The hotter it gets, the more violent the reaction becomes. Other sacrificial metals that are used to cement precious metals is iron and aluminum. Iron can be obtained through bare steel scrap metal. It leaves a dirty solution as it will cement nearly every metal in the reactivity series. But, you will be sure to get all metals out. Aluminum will react the same way zinc does. Aluminum will create a filtering problem by the nature of the metal. Aluminum chloride is a gelatinous mass in solution, depending on amount dissolved, and will clog filters that seemingly looks empty. Each one has it's pro's and con's. You have to safely experiment and see which is best for your particular needs.


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## Geo

Lars100 said:


> Hello !
> Soo many thanks !!!
> I believe I got the hang of it and have made it quite succesfully to -"The sollution should be some color of red". That is exactly what I´m having ! And I tried to get rid of de silver just by decant/siphon it. But now... -"Precipitating the Pd with ammonium chloride + chlorine gas will give you a red salt of Pd" sounds very scary to me...(even me...) ! Chlorine gas ? How can I work with Chlorine gas ? Sounds better to -"cement onto copper to obtain a slightly impure palladium metal in one go". But how does it work (I have never done it) ? Do I just put sticks of copper into the fluid and wait for it to stick ? For how long ? How can i be sure to get it all ? And wont the copper disolve into the acid ?
> Sorry for all my questions...but I think I got the red fluid right and I don´t want to spoil it all now...


The chlorine gas can be produced in situ. If I am in a hurry (bad idea any time) instead of setting up a chlorine generator by decomposing sodium chloride in sulfuric acid and bubbling the resulting gas through the solution, I just sprinkle in some trichloro pool chlorinator. It comes in a solid "puck" or powder. I use the powder. This is not a chemical where more is less. This is a chemical where a little goes a long way. By reading the label, most trichloro up in the high 90% pure chlorine. It will dissolve in acidic solution producing copious amounts of chlorine gas. After adding the ammonium chloride, add just a pinch and stir it in well. The red salt will start forming. You can't get it all this way. There is a certain balance that will be maintained in the solution that is determined by the volume of liquid. The more free liquid available, the more Pd that will be left in solution so it's always better to work with a concentrated solution.


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## Lars100

Hi Orvi !
Thanks for input !
And I fully understand. I only work in batches that I can handle. Been working with about 600g MLCCS per shot.
What I mean with "solid process" is simply that I will finish the whole lot into the "burgundy red fluid" + silver and then READ and LEARN how to move forward (yes, test the batch also).
I must find a way which I then (rather easily - hopefully) can "copy/paste" over and over until I've processed it all.


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## Lars100

Many thanks Geo !
This sounds like a path forward. I will study it more.
- But it still looks like I will end up with a "mix of metals" in the ready soup.
We can discuss this later when Ive tested a bit but my big concern is how to


Geo said:


> I use copper when copper is already in the solution. The "go to" when cementing PGM's is normally zinc powder or turnings. Add small amounts incrementally as the reaction is exothermic and can get out of hand quickly. The reaction is complete when the solution loses all color except maybe a light green tint that will not cement out, The hotter it gets, the more violent the reaction becomes. Other sacrificial metals that are used to cement precious metals is iron and aluminum. Iron can be obtained through bare steel scrap metal. It leaves a dirty solution as it will cement nearly every metal in the reactivity series. But, you will be sure to get all metals out. Aluminum will react the same way zinc does. Aluminum will create a filtering problem by the nature of the metal. Aluminum chloride is a gelatinous mass in solution, depending on amount dissolved, and will clog filters that seemingly looks empty. Each one has it's pro's and con's. You have to safely experiment and see which is best for your particular needs.



separate and refine the PD ?


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## kurtak

Lars100 said:


> What I mean with "solid process" is simply that I will finish the whole lot into the "burgundy red fluid" + silver *and then READ and LEARN how to move forward*


Per the bold print (in above quote) --- you have it all wrong - as in you have it backwards - you are putting the cart before the horse

When working with PGMs (Platinum Group Metals) including Pd - you do NOT go putting the PGMs into solution first --- & then READ & LEARN how to move forward

You READ & LEARN *FIRST *- then start working on putting the - "lot into the "burgundy red fluid"

Working with recovery & refining of PGMS is a *EXTREMLY RISKY & TOXIC* process - you are working with *POISON*

PGM POISONING is very much like lead or mercury poisoning - it doesn't kill you right away (today - tomorrow - this month - next month - this year &/or even next year) that is because it gets in your system/body *& STAYS there* & starts killing you over time - which can be several years 

A few things to know/understand about platinum (GROUP metal) poisoning/toxicity -------

platinum (group metals) toxicity vary depending on the amount you are currently exposed to, which can/will lead to the following


Allergic reactions of the skin & or mucous membranes
*Kidney disease’s*
*Intestinal & digestive problems*
*Muscle spasms*
*High blood pressure* (Hypertension)
Deafness
*Cancer*

*Everyone* that has been trying to help you here has tried to *WARN* you about this & has tried to tell you that the *VERY FIRST* thing you *MUST* do is LEARN & READ - and THEN set up to do this *SAFELY* - then - and only then - put "the whole lot into the "burgundy red fluid"

If you do not follow this advise to FIRST - get everything you *NEED* to do this safely - & then set up to do this safely - *YOU ARE GOING TO POISON YOURSELF* - AND POISON EVERYONE that comes into your back yard where you are doing this

*PLEASE* put what you are doing off to the side & *STOP *what you are doing - until you *FULLY* understand how to do this safely AND set up to do this safely

*We can & will help you with this *(setting up to do it safely)

*Other wise you are on a path to self destruction - you just don't realize it because you are blinded by the high price of a small amount of metal*

Edit to add; - I just hope - that with the way you are currently going about this that you don't have a wife & kids around what you are doing - because if you do - you are POISONING then to

Kurt


----------



## kurtak

One more thing - just because you see others - on YouTube - that don't know any better - doing stupid stuff - doesn't mean you have to be stupid to 


We are here to help you from being stupid

Kurt


----------



## MicheleM

@Lars100 in my opinion working with " 600 g for shot" is too much for a beginner. You should try with a smaller batch, around 50 g , random sorted. They generate a lot of acidic liquid waste. All this without mentioning that this is a very dangerous activity, with around 50 g, is more manageable, and in the end you will decide what to do with the rest of them.


----------



## Lars100

Hi Kurt !
Many thanks for Your concern.
- To reach the level of "burgundy red fluid" I believe I have worked out a safe process. I´m done up to 95% and just finishing up the rest.
The fluids are put away nicely in bottles.

But You are correct. I am a bit worried about the next steps (safety, process and refining


kurtak said:


> Per the bold print (in above quote) --- you have it all wrong - as in you have it backwards - you are putting the cart before the horse
> 
> When working with PGMs (Platinum Group Metals) including Pd - you do NOT go putting the PGMs into solution first --- & then READ & LEARN how to move forward
> 
> You READ & LEARN *FIRST *- then start working on putting the - "lot into the "burgundy red fluid"
> 
> Working with recovery & refining of PGMS is a *EXTREMLY RISKY & TOXIC* process - you are working with *POISON*
> 
> PGM POISONING is very much like lead or mercury poisoning - it doesn't kill you right away (today - tomorrow - this month - next month - this year &/or even next year) that is because it gets in your system/body *& STAYS there* & starts killing you over time - which can be several years
> 
> A few things to know/understand about platinum (GROUP metal) poisoning/toxicity -------
> 
> platinum (group metals) toxicity vary depending on the amount you are currently exposed to, which can/will lead to the following
> 
> 
> Allergic reactions of the skin & or mucous membranes
> *Kidney disease’s*
> *Intestinal & digestive problems*
> *Muscle spasms*
> *High blood pressure* (Hypertension)
> Deafness
> *Cancer*
> 
> *Everyone* that has been trying to help you here has tried to *WARN* you about this & has tried to tell you that the *VERY FIRST* thing you *MUST* do is LEARN & READ - and THEN set up to do this *SAFELY* - then - and only then - put "the whole lot into the "burgundy red fluid"
> 
> If you do not follow this advise to FIRST - get everything you *NEED* to do this safely - & then set up to do this safely - *YOU ARE GOING TO POISON YOURSELF* - AND POISON EVERYONE that comes into your back yard where you are doing this
> 
> *PLEASE* put what you are doing off to the side & *STOP *what you are doing - until you *FULLY* understand how to do this safely AND set up to do this safely
> 
> *We can & will help you with this *(setting up to do it safely)
> 
> *Other wise you are on a path to self destruction - you just don't realize it because you are blinded by the high price of a small amount of metal*
> 
> Edit to add; - I just hope - that with the way you are currently going about this that you don't have a wife & kids around what you are doing - because if you do - you are POISONING then to
> 
> Kurt



) and that´s why Im writing here on the forum.


----------



## Lars100

Dear Michele (and Kurt),
At this time I dont think I dare to tell you in detail what Ive done so far.
- But I found a workable way to come to this point.
Basically I added 0.4L Nitric acid to the "tin free" 600g MLCCs. Let them stay so for a week (just rotated and mixed well a couple of times).
- It was bad if I let them stay longer as it resulted in thick cream (impossible/very hard to filter).
After a week I decanted and filtered. Components/mass in a "big box" (still there...maybe a 2nd round later ?) and the black/green fluid into bottles.
Added about 0.3dl of HCL and waited overnight. 
The fluid changed color into "burgundy red" and with a white/beige/red layer at the bottom (silver ?).
Decant/siphon/separated the white from the red. Thats where we are today.
Im still waiting for my tin so I can make stannous test.


MicheleM said:


> @Lars100 in my opinion working with " 600 g for shot" is too much for a beginner. You should try with a smaller batch, around 50 g , random sorted. They generate a lot of acidic liquid waste. All this without mentioning that this is a very dangerous activity, with around 50 g, is more manageable, and in the end you will decide what to do with the rest of them.


----------



## Geo

@Lars100
I concur with Kurt. Storing ionized Pd is a dangerous situation. Accidents happens, an act of god, an earthquake or storm. It's better to keep that kind of toxin in metallic form until you are ready to go from start to finish. This reduces the time that the metal is most deadly. There was two great people from this forum that I knew personally, and a third that's suspected, that has died from complications of platinosis.
Since the Pd came from MLCC's, it should be pretty pure as it is. Move the solution to a large enough beaker to hold the solution and still have 2/3 to 3/4 of the volume empty. Add 50ml's of HCl to drop the silver as silver chloride. Filter the silver out and replace the solution to the beaker. Dilute the solution to double it's volume. Start adding small amount of steel wool while stirring. The steel wool will have the tendency to float. It needs to stay submerged as much as possible. This will produce a small amount of aerosol from the reaction, so wear gloves and a mask if you are not working in a fume hood. Keep adding the steel wool until the solution loses it's red color and turns slightly green. It will produce a light, fluffy black powder. You may see small bits of steel wool that does not react. Don't be alarmed as steel contains carbon. What you are seeing will be the carbon retaining the shape. It is of no consequence to the recovery or melting of the powder. Ideally, you would continue adding steel until you get a negative stannous chloride test result. You will have to settle for a colorless solution except for the before mentioned light green color. Filter all black powder out of solution. Now you have a mostly purified black powder of Pd called (PGM blacks). You can melt as is or store and add more to it later. Don't be surprised at the volume of the black powder. It makes a huge volume of powder that dries to a much smaller mass. It dries up next to nothing to be honest. It will make you think it evaporated off but that's just the nature of cemented powder. Now your palladium is much less dangerous than it was as a liquid. The powder will be very fine and light and can be lifted into the air by a small puff of wind. The black powder is still just as toxic as the liquid so take great care to capture all of the powder and store it damp until you are ready to melt it.


----------



## Geo

For tin, go to your local walmart and buy lead free fishing weights. The pure tin "split weights" will be a lustrous white metal that will look like silver. Also, lead free tire weights is pure tin. If you have to order tin to make stannous chloride, you can just buy stannous chloride crystals from Amazon or Ebay. Just add water to the crystals and allow them to dissolve. Keep solution away from heat and strong light (sunshine) to keep it fresh longer.


----------



## Lars100

Dear Geo,
This was really exciting to read and a process that I should be able to handle.
I will definitely test this.
Again, stannous test next week and then also bring together the parts needed to make a first try with Your methode.
Thanks !
Ps. I got many litres of that deep Burgundy red fluid so you can understand I need a workable methode.


----------



## Lars100

Geo said:


> @Lars100
> I concur with Kurt. Storing ionized Pd is a dangerous situation. Accidents happens, an act of god, an earthquake or storm. It's better to keep that kind of toxin in metallic form until you are ready to go from start to finish. This reduces the time that the metal is most deadly. There was two great people from this forum that I knew personally, and a third that's suspected, that has died from complications of platinosis.
> Since the Pd came from MLCC's, it should be pretty pure as it is. Move the solution to a large enough beaker to hold the solution and still have 2/3 to 3/4 of the volume empty. Add 50ml's of HCl to drop the silver as silver chloride. Filter the silver out and replace the solution to the beaker. Dilute the solution to double it's volume. Start adding small amount of steel wool while stirring. The steel wool will have the tendency to float. It needs to stay submerged as much as possible. This will produce a small amount of aerosol from the reaction, so wear gloves and a mask if you are not working in a fume hood. Keep adding the steel wool until the solution loses it's red color and turns slightly green. It will produce a light, fluffy black powder. You may see small bits of steel wool that does not react. Don't be alarmed as steel contains carbon. What you are seeing will be the carbon retaining the shape. It is of no consequence to the recovery or melting of the powder. Ideally, you would continue adding steel until you get a negative stannous chloride test result. You will have to settle for a colorless solution except for the before mentioned light green color. Filter all black powder out of solution. Now you have a mostly purified black powder of Pd called (PGM blacks). You can melt as is or store and add more to it later. Don't be surprised at the volume of the black powder. It makes a huge volume of powder that dries to a much smaller mass. It dries up next to nothing to be honest. It will make you think it evaporated off but that's just the nature of cemented powder. Now your palladium is much less dangerous than it was as a liquid. The powder will be very fine and light and can be lifted into the air by a small puff of wind. The black powder is still just as toxic as the liquid so take great care to capture all of the powder and store it damp until you are ready to melt it.


Again, many thanks for this advice. Im just about to order some steel-wool but there seem to be various qualities (like fine or rough). Any sugestions ?
And you say -"Dilute the solution to double it's volume". Shall I do that with dl water ?
And the silver already been separated (we can discuss about how to refine that one also...).
- Now, Im still waiting for my tin to do the stannous but I can start testing with the steel-wool if that comes first.
- Im a bit worried that I havent got all the good things out of the MLCCs (after decante out the Nitric acid).
I took a part and added HCL. The mass/fluid immediately changed color to orange/red. So there seems to something good still there...
Again, many thanks (so far) !
Lars


----------



## Geo

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.


----------



## dpgold

Lars100 said:


> Thanks for input !
> Ehh...Stannous-test...how do I perform such a test ?
> Air-bubbler ? Any brand, type You can recommend ?


it is a liquid comprised of TIN and HCL, I am not sure about the exact proportions but seems like 12g fine grinded TIN or TIN powder dissolved in HCL about 50ml (Muriatic acid concentration) it takes a while to dissolve. Kept in a dark bottle and is good only for a couple of months. If the solution contains PGM or gold it will change color on the test strip. Soak a test strip in the solution which you believe contains these metals dissolved and then put a tiny drop of Stannous solution on it. Depending on the metals contained and concentration the strip will change color indicating their presence


----------



## kurtak

Geo said:


> 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.


This is one of those things where the old saying - "there is more then one way to skin a cat" - is true



Geo said:


> When wet processing, the ceramic bodies have to break down into dust to get a complete leaching.


This is true - in order to leach all the Ag/Pd out of the ceramic bodies of MLCCs the ceramic bodies need to be broke down to the "fine" silt/dust - which will put (dissolve) all the Ag/Pd into the nitric leach solution

Edit to add; - other wise all you are really going to get is the Ag/Pd on each "end" of the MLCC

The problem with "leaching" MLCCs is getting *all* of the leach out of that "fine" silt/dust - it's like "fine" clay which is next to impossible (*if not impossible*) to filter --- &/or wash out

Because filtering is "impossible" --- decanting - washing - settling - multiple times is really the only way to get "*most*" of the leach out of the silt dust --- I say most - because even with washing you won't get it all - there will *always* be at least *traces* (or more) left in the silt/dust (depending on amount of washing) you just can't get it all - which (with all the washing) will give you a VERY dilute leach solution

Then - after all the washing - you will likely need to do some (or a lot) evaporation to concentrate the leach back down - otherwise the silver (chloride) & then the Pd will come down ultra fine - making washing/filtering those precipitates difficult

At least that was my experience the first (and one & only) time I tried leaching MLCCs - what a pain in the butt - so much so that I decided that I would never again leach MLCCs

IMO - if you are going to process MLLCs - smelting is the way to go - they still need to be milled to a "fine" dust so that the alumina (ceramic) will slag off AND you need to use cryolite as "part" of your flux make up as cryolite dissolves the alumina allowing it to slag off

Flux for smelting MLCCs - 1/3 borax 1/3 soda ash 1/3 cryolite & "some" fluorspar for thinning

If you do a HIGH temp roast (get them "red" hot) on the MLCCs before milling they will mill easier & more completely to the dust you are looking for

Edit to add; - once red hot let them roast for "at least" one hour - if not two 

Use silver as your collector metal in the smelt - then process you dore with nitric - proceed with dropping silver chloride (as normal) then Pd recovery (cementing with copper recommended)

As I said - "more then one way to skin a cat" 

Kurt


----------



## jphayesjr

Thanks for the suggestions. I have 25 kilos of old MLCCs, and am in process of planning the refining project. I have technical reasons to believe the material will contain significant AU, PT, RH, as well as AG and PD. Any suggestions how to proceed stepwise to recover all?


----------



## jphayesjr

jphayesjr said:


> Thanks for the suggestions. I have 25 kilos of old MLCCs, and am in process of planning the refining project. I have technical reasons to believe the material will contain significant AU, PT, RH, as well as AG and PD. Any suggestions how to proceed stepwise to recover all?


Should add, I'll be getting up to75 k more soon, all from a defunct repair company on original reels, will be looking into professional refiners. The engineers out there know how a scaled up process will differ from benchtop assay methods. I know I need to have a good grasp of the processes and chemical equations involved for all the best reasons, to choose someone who offers the best options.


----------



## Yggdrasil

jphayesjr said:


> Thanks for the suggestions. I have 25 kilos of old MLCCs, and am in process of planning the refining project. I have technical reasons to believe the material will contain significant AU, PT, RH, as well as AG and PD. Any suggestions how to proceed stepwise to recover all?


I would expect, if lucky to have significant amount of Ag and Pd in there, the rest is just scam food, which make me think the start is a scam.
There is and have never been, as far as I know, anything else of value, than AG and Pd in high grade MLCCs


----------



## orvi

Yggdrasil said:


> I would expect, if lucky to have significant amount of Ag and Pd in there, the rest ia just scam food, which make me think the start is a scam.
> Ther is and have never been, as far as I know, anything else of value, than AG and Pd in high grade MLCCs


Maybe some super-fancy with gold plated ends  I also do not know what else should be in there. Old Soviet MLCCs sometimes used platinum, not palladium. Some batches of mixed MLCCs gave even 50/50 PtPd mix. Never heard about Rh or gold inside. But in modern stuff... I doubt even about palladium. From the point when sinter technology for nickel developed for MLCCs, Pd ones are very scarce.


----------



## kurtak

jphayesjr said:


> I have technical reasons to believe the material will contain significant AU, PT, RH, as well as AG and PD


Not sure where you heard that MLCCs have Au Pt or Rh in them (although I have seen "some" with gold "plating" on the ends - but - they are rare)

OLD MLCCs were made with Pd/Ag

Or as orvi said (old) Soviet made stuff will have Pt in place of the Pd

There are two types of MLCCs - NME (Noble Metal Electrode) MLCCS --- & (BME Base Metal Electrode)

NME MLCCS are made of Ag/Pd (the exception being Soviet stuff with Pt in place of Pd)

BME MLCCS are made of copper & nickel

In the "late' 1990s (around 1997) because of the "rising" price of noble metals - & the cost of making NME MLCCS going up significantly the quite making NME MLCCs & started making BME MLCCs

So after (around 1997) the *VAST majority* of MLCCs are made of copper/nickel *NOT* Ag/Pd

There is an easy why to test if MLCCS are made of base metals - or made of noble metals

Nickle is magnetic - so a magnet will pick up BME MLCCS because of the 50% nickel alloyed with the copper - but a magnet will not pick up NME MLCCs as Ag &Pd are not magnetic


jphayesjr said:


> Should add, I'll be getting up to75 k more soon,


My point is - if you are "buying" these * make sure you use your magnet* BEFORE paying for these or you will be very disappointed when you get them & find out they are made of Cu/Ni & not mad of Ag/Pd

If you can't test them with a magnet - before buying them - I would walk away as it "may" be a scam

Not saying it is - just warning you to be careful as these kind of scams *happen all the time*

Kurt


----------



## kurtak

One more note - you said ---------



jphayesjr said:


> I have technical reasons to believe the material will contain significant AU, PT, RH, as well as AG and PD


If it is the seller telling you all those metals are in MLCCs* you are more then likely being scammed *

There is *NO* Rh in MLCCs

Au *ONLY* if they are "plated" on the ends (which is rare)

Pt *ONLY* if they are OLD Soviet MLCCs

Ag/Pd if made BEFORE 1997 - if made AFTER 1997 *MOST likely* Cu/Ni

Kurt


----------



## Lars100

jphayesjr said:


> Thanks for the suggestions. I have 25 kilos of old MLCCs, and am in process of planning the refining project. I have technical reasons to believe the material will contain significant AU, PT, RH, as well as AG and PD. Any suggestions how to proceed stepwise to recover all?


Hello there !
I have done about 30kg but Im not at the end yet. I believe I have some good ideas to share...but...I will hold back a little as I don´t now if it will work out. See my comments to Geo ! I will tell when I´m succesful (or just fade away if I don´t...) !


----------



## Lars100

Geo said:


> @Lars100
> I concur with Kurt. Storing ionized Pd is a dangerous situation. Accidents happens, an act of god, an earthquake or storm. It's better to keep that kind of toxin in metallic form until you are ready to go from start to finish. This reduces the time that the metal is most deadly. There was two great people from this forum that I knew personally, and a third that's suspected, that has died from complications of platinosis.
> Since the Pd came from MLCC's, it should be pretty pure as it is. Move the solution to a large enough beaker to hold the solution and still have 2/3 to 3/4 of the volume empty. Add 50ml's of HCl to drop the silver as silver chloride. Filter the silver out and replace the solution to the beaker. Dilute the solution to double it's volume. Start adding small amount of steel wool while stirring. The steel wool will have the tendency to float. It needs to stay submerged as much as possible. This will produce a small amount of aerosol from the reaction, so wear gloves and a mask if you are not working in a fume hood. Keep adding the steel wool until the solution loses it's red color and turns slightly green. It will produce a light, fluffy black powder. You may see small bits of steel wool that does not react. Don't be alarmed as steel contains carbon. What you are seeing will be the carbon retaining the shape. It is of no consequence to the recovery or melting of the powder. Ideally, you would continue adding steel until you get a negative stannous chloride test result. You will have to settle for a colorless solution except for the before mentioned light green color. Filter all black powder out of solution. Now you have a mostly purified black powder of Pd called (PGM blacks). You can melt as is or store and add more to it later. Don't be surprised at the volume of the black powder. It makes a huge volume of powder that dries to a much smaller mass. It dries up next to nothing to be honest. It will make you think it evaporated off but that's just the nature of cemented powder. Now your palladium is much less dangerous than it was as a liquid. The powder will be very fine and light and can be lifted into the air by a small puff of wind. The black powder is still just as toxic as the liquid so take great care to capture all of the powder and store it damp until you are ready to melt it.


Hi Geo !
Now I´m a bit further ! Stannous test has been performed with good results and happily I started with the next step.
In short, there was a rather huge reaction when I started to add steel wool and for just a short while it turned towards green but then the bubbles started to become brown and brown they stayed. 
After finish it I filtered it and the brown mass stayed in the filter while I got a black liquid with a shimmering fluid on the surface in the beaker. I did another sample in which Im pretty certain there were no silver at all remaining in the fluid. But same result. 
Please see attached pic of a stannous test of a sample. Does it say anything ? Strip is dark brown and the filter-paper is orange/black/greenish...


----------



## kurtak

Lars100 said:


> Please see attached pic of a stannous test of a sample.


Is that the stannous test before - or after putting the steel wool in your solution ?

Kurt


----------



## kurtak

Lars100 said:


> After finish it I filtered it and the brown mass stayed in the filter


I could be wrong - but - it sounds like the steel wool cemented copper

Which would be the case IF (the BIG IF) the MLCCS were BME MLCCS instead of NME MLCCs

Cemented Pd should be a "dark" gray to black - not brown

Can you post a pic of the brown mass that stayed in your filter ?

Kurt


----------



## kurtak

Lars100 said:


> I will tell when I´m succesful (*or just fade away if I don´t*...) !


Per the bold print - *please* - whether you have good results - or - bad results - post your results

posting bad results is just as important as posting good results as even bad results is part of the learning/teaching process --- which is what the purpose of this forum is (learning/teaching)

Edit to add; - when I first started to learn about refining - I had to post about *A LOT* of bad results - that is how I learned to get good results 

Kurt


----------



## Geo

pH plays a part in successfully cementing Pd. If the solution is acidic enough, the finely divided Pd will simply redissolve after the steel wool is depleted. There are two easy ways to help the process. Dilute the solution with water or raise the pH by adding hydroxide or carbonate dissolved in water to the solution in small increments. Unless you have done other processes with the solution since the leaching process, the solution will most likely have a pH of 0. You want to adjust it up to 2. If the solution is saturated with metal salt, this will cause some oxides to form. But again, Pd will not leave the solution easily. As you are adding the base, watch for a cloud to form in the solution. It should redissolve on it's own if you are doing the additions and stirring correctly. Stop adding the base when a cloud forms and does not redissolve in a few minutes time. Filter the solution and cement again. Ideally, you want the steel wool to neutralize the solution to the point that the Pd does not redissolve. If you have 1000mls of solution and for what ever reason you can't get anything to work right, dump it in a bucket and add a gallon of water. Now it will cement on iron and will not go back into solution so fast that you can't collect the powder. This creates a lot of liquid waste and should be avoided if at all possible.


----------



## Lars100

kurtak said:


> Is that the stannous test before - or after putting the steel wool in your solution ?
> 
> Kurt


Hi Kurt !
Thanks for taking time with this.
- I will take some more pictures tomorrow showing stannous and what samples I took/and what I did.
Thanks for Your patience.
Br Lars


----------



## Lars100

Geo said:


> pH plays a part in successfully cementing Pd. If the solution is acidic enough, the finely divided Pd will simply redissolve after the steel wool is depleted. There are two easy ways to help the process. Dilute the solution with water or raise the pH by adding hydroxide or carbonate dissolved in water to the solution in small increments. Unless you have done other processes with the solution since the leaching process, the solution will most likely have a pH of 0. You want to adjust it up to 2. If the solution is saturated with metal salt, this will cause some oxides to form. But again, Pd will not leave the solution easily. As you are adding the base, watch for a cloud to form in the solution. It should redissolve on it's own if you are doing the additions and stirring correctly. Stop adding the base when a cloud forms and does not redissolve in a few minutes time. Filter the solution and cement again. Ideally, you want the steel wool to neutralize the solution to the point that the Pd does not redissolve. If you have 1000mls of solution and for what ever reason you can't get anything to work right, dump it in a bucket and add a gallon of water. Now it will cement on iron and will not go back into solution so fast that you can't collect the powder. This creates a lot of liquid waste and should be avoided if at all possible.


Thanks Geo !
Im so glad that You have answers for me. I will go back tomorrow and take some more pics. I was suspecting that my mixture is wrong. Im pretty sure I have to much acid for ex. I added the same amount of diluted water to the fluid and then started to feed with steel-wool...well...it boils and smoke (yes, I was prepared for it). It calmed down and I added more steel-wool...new boiling session...and so on a couple of times until the steel-wool didn´t react anymore.
Pictures are coming tomorrow...
But one question here...adding the steel wool...in the best scenario I will end up with steel and PD, right ? How will I get rid of the steel ?


----------



## Geo

Lars100 said:


> Thanks Geo !
> Im so glad that You have answers for me. I will go back tomorrow and take some more pics. I was suspecting that my mixture is wrong. Im pretty sure I have to much acid for ex. I added the same amount of diluted water to the fluid and then started to feed with steel-wool...well...it boils and smoke (yes, I was prepared for it). It calmed down and I added more steel-wool...new boiling session...and so on a couple of times until the steel-wool didn´t react anymore.
> Pictures are coming tomorrow...
> But one question here...adding the steel wool...in the best scenario I will end up with steel and PD, right ? How will I get rid of the steel ?


The dissolved steel will not be an issue. It will stay in solution until the solution is completely neutralized. Any metallic steel left can be removed with a magnet. There will be a noticeable amount of carbon left behind from the steel. Steel is a man made metal. It is created by mixing iron and carbon primarily. Steel is a soft metal compared to iron. Iron has a crystalline structure that makes iron very hard, but brittle. Other additives gives it different properties. Iron can not be cemented from solution. Once it's dissolved, it's locked in the solution and can not effect future processing with the simple processes we use. The carbon left behind from the steel will convert to carbon dioxide well before PGM's melt.


----------



## Lars100

Dear all,
So, please see attached pics. Pictures showing what I got and then I do stannous test. First pictures show "the mass I got when adding steel wool to my acid fluids (filtered MLCC solution after being in Nitric acid and then silver separated with HCL -see earlier comments). I added extra steel wool in the end of the process and let it stay overnight. It turned out the the process wasn´t finished so that steel wool dissolved to. Pic 2 shows after stiring it together. The mass blackened but I must say it´s still more brown (pic2).
I filtered the lot I made last week (same procedure) and the filterer "steel wool" can be seen in Pic 3.
I used another method earlier (from Youtube) where I neutralized the acid with Sodium carbonate (pic 4) and pic 5 shows the result after boiling it down.

Stannoust testing.
Pic6 shows the setup of above samples. Pic 7. shows the result after just adding the stannous fluid (30sec). Pic 8 after 2 min and Pic 9 after 5 min.
I look forward to hear Your comments/conclusions of it all !


----------



## Lars100

Geo said:


> The dissolved steel will not be an issue. It will stay in solution until the solution is completely neutralized. Any metallic steel left can be removed with a magnet. There will be a noticeable amount of carbon left behind from the steel. Steel is a man made metal. It is created by mixing iron and carbon primarily. Steel is a soft metal compared to iron. Iron has a crystalline structure that makes iron very hard, but brittle. Other additives gives it different properties. Iron can not be cemented from solution. Once it's dissolved, it's locked in the solution and can not effect future processing with the simple processes we use. The carbon left behind from the steel will convert to carbon dioxide well before PGM's melt.


Geo, ah a magnet !!! The easiest is the best !!! Now I can only hope I got the "right stuff". Please see my new inlay !
Many thanks for sharing Your knowledge and experience !


----------



## Lars100

kurtak said:


> Per the bold print - *please* - whether you have good results - or - bad results - post your results
> 
> posting bad results is just as important as posting good results as even bad results is part of the learning/teaching process --- which is what the purpose of this forum is (learning/teaching)
> 
> Edit to add; - when I first started to learn about refining - I had to post about *A LOT* of bad results - that is how I learned to get good results
> 
> Kurt


Thanks Kurt !
Yes, I know...I get super frustrated when I read a thread (about anything) and it ends up in nothing. Either the problem has been solved or not... The person in charge of the thread is gone...happy with a solution he/she didn´t share or just sad with an unsolved issue...
- Today I´ve made a new post. I look forward to hear Your thoughts of it !
Br - Lars


----------



## jphayesjr

Thanks for the tips, the reels on which some of my MLCCs came indicate they contain the other PGM, and yes, some have gold or Pt/Pd plated caps. These were used yo repair civilian radios, avionics, radars, sonar, and yes, they are rare.


----------



## jphayesjr

orvi said:


> Maybe some super-fancy with gold plated ends  I also do not know what else should be in there. Old Soviet MLCCs sometimes used platinum, not palladium. Some batches of mixed MLCCs gave even 50/50 PtPd mix. Never heard about Rh or gold inside. But in modern stuff... I doubt even about palladium. From the point when sinter technology for nickel developed for MLCCs, Pd ones are very scarce.


During the 1980s and 1990s, Rh was often not even refined out of other PGMs, or gold or silver, it was a cheaper substitute for PT/Pd, it's only large scale commercial use was anti-corrosive plating on silver, especially jewelry.


----------



## kurtak

Geo said:


> pH plays a part in successfully cementing Pd. If the solution is acidic enough, the finely divided Pd will simply redissolve after the steel wool is depleted.


Geo - I am sorry but this simply is not true - Ph plays little or no role in cementing Pd from an acidic solution 

At least not in a nitric solution or an AR solution 

*There is one exception* to that & that is when Pd is dissolved in CuCl2 - when Pd is dissolved in CuCl2 you get PdCl2 --- CuCl2 & PdCl2 are *Co-catalyst* --- so - during the reaction (when trying to cement Pd from CuCl2) PdCl2 is reduced to Pd - and then the CuCl2 serves to re-oxidize (redissolve) this back to PdCl2. Air can then oxidize the resultant CuCl back to CuCl2, completing the cycle. 

This makes cementing Pd from a CuCl2 solution very difficult - therefore - yes - in the case of Pd dissolved in CuCl2 you may well have to adjust Ph (up) in order to overcome the Co-catalyst cycle (PdCl2 being reduced to Pd by cementing - the CuCl2 redissolving the Pd to PdCl2 - in a continuing ongoing cycle)

Pd dissolved in a nitric &/or AR can be cemented form those solutions - directly - without the need to dilute &/or adjust Ph --- & cementing with copper is the preferred metal for doing the cementing 

Cementing PGMs (including Pd) with copper - from nitric & AR - has been a long standing "standard" in LARGE scale refineries forever & they do so without the need to adjust Ph

They use copper to cement PGMs from AR after dropping the gold in AR solutions that also have PGMs in them

The same holds true (cementing with copper - without the need to adjust Ph) in nitric solutions that have PGMs dissolved in them

The fact of the matter is - you can cement Pd directly from a "concentrated" nitric or AR solution --- however - diluting the solutions - "a little" (like two or three times) does not hurt - but you most certainly do not have to dilute so much as to change the Ph by a factor of 2 --- in fact doing so will dilute it so much it (the Pd) will come down "ultra " fine --- not a good thing

To put that (diluting to change Ph) in perspective --------

To change Ph from 0 to 1 --- you have to dilute 10 times --- that means you would have to dilute 1 liter to 10 liters

To change Ph from 0 to 2 --- you have to dilute 100 time --- that means you would have to dilute 1 liter to 100 liters

To change Ph from 0 to 3 --- you have to dilute 1000 times --- that means you would have to dilute 1 liter to 1000 liters 

That is a LOT of diluting - even to change Ph from 0 to 1 - & it is not necessary

Adjusting Ph with a base also in not necessary - nor do you want to do so - if you don't need to - it can & is likely to lead to "other" complications 

Cementing with iron is a *VERY* dirty/messy way of going about this when it can be done with copper resulting in *MUCH *cleaner cementing 

Bottom line - there are simpler & "cleaner" ways to get this done

Kurt


----------



## jphayesjr

jphayesjr said:


> Should add, I'll be getting up to75 k more soon, all from a defunct repair company on original reels, will be looking into professional refiners. The engineers out there know how a scaled up process will differ from benchtop assay methods. I know I need to have a good grasp of the processes and chemical equations involved for all the best reasons, to choose someone who offers the best options.


An image of one of literally trunks full, price was retail for reel in-trade only...coding on obverse indicates they were made in late 80s to early 90s


----------



## Lars100

kurtak said:


> I could be wrong - but - it sounds like the steel wool cemented copper
> 
> Which would be the case IF (the BIG IF) the MLCCS were BME MLCCS instead of NME MLCCs
> 
> Cemented Pd should be a "dark" gray to black - not brown
> 
> Can you post a pic of the brown mass that stayed in your filter ?
> 
> Kurt


Hello Kurt !
I believe You have a point here. All the MLCC´s I got are from 2005 or older and about 50% are coming from Samsung. According to their own specification from that time they say that the inner electrode is made of Ni or Pd. The outer electrode consist of three layers made of Cu or Ag (inner), Ni (middle) and Sn/Pb (outer). We had the components laying in 15% HCL for a week to wash away the outer layer and I believe we were fairly succesful in doing that (outside layer diminished and changed color).
- I will post some more pics of the "brown mass" shortly !!!
Thanks for Your time and good ideas !


----------



## Lars100

Lars100 said:


> Hello Kurt !
> I believe You have a point here. All the MLCC´s I got are from 2005 or older and about 50% are coming from Samsung. According to their own specification from that time they say that the inner electrode is made of Ni or Pd. The outer electrode consist of three layers made of Cu or Ag (inner), Ni (middle) and Sn/Pb (outer). We had the components laying in 15% HCL for a week to wash away the outer layer and I believe we were fairly succesful in doing that (outside layer diminished and changed color).
> - I will post some more pics of the "brown mass" shortly !!!
> Thanks for Your time and good ideas !


Hello again !
Please see attached pics. I didn´t "feed" the first batch so well with steel wool so it was very "wet". I filtered it and as You can see the filter is very brown while the liquid is green/black.
In the second batch I had more steel wool so it became a thicker mass (no running fluid). To my surprise the top layer is very brown while the underneath mass is more black/grey but is has indeed also a lot of brownish in it.


----------



## kurtak

Lars100 said:


> Hello again !
> Please see attached pics. I didn´t "feed" the first batch so well with steel wool so it was very "wet". I filtered it and as You can see the filter is very brown while the liquid is green/black.
> In the second batch I had more steel wool so it became a thicker mass (no running fluid). To my surprise the top layer is very brown while the underneath mass is more black/grey but is has indeed also a lot of brownish in it.


Please *STOP* what you are doing - you are creating *MESSES* that we are now (likely) going to have to clean up

I say likely clean up because IF (the BIG IF) there was actually Pd in your solution(s) that Pd is now likely tied up in that brown mass - so now we will likely need to clean that up

That brown mass is iron oxide (basically rust) as a result of using steel wool in a nitric solution

Put those filters in a plastic container with a lid on them so they don't dry out (we "may" need to come back to them)

Put the solutions aside until we are able to discuss this in more detail --- in other words - slow down & in fact stop until "others" have chimed in - instead of just jumping in on the advice of one person

I say that because "sometimes" there are mis-understandings in what is posted - which may (or not) lead to mistakes made in the advice given - so it is always good to "wait" & hear what others have to say as someone else may catch the mis-understanding & correct it

I believe that is the situation here

Steel wool does not work well in a nitric solution (which is what you have) & we are now seeing the results of that

Steel wool is better suited with HCl solutions

So Geo did not give bad advice - I "think" he just mis-understood your situation --- waiting for "others" to chime in "may" have avoided the mess(es) you have now created

Trust me - I to sometime mis-understand what I read - post a reply - & then someone else has to correct me

My point being - as someone still learning - slow down & wait for others to chime in so that discussions are more complete - instead of just jumping in on the advice of "one" post

To be continued (all I have time for today)

Kurt


----------



## Lars100

kurtak said:


> Please *STOP* what you are doing - you are creating *MESSES* that we are now (likely) going to have to clean up
> 
> I say likely clean up because IF (the BIG IF) there was actually Pd in your solution(s) that Pd is now likely tied up in that brown mass - so now we will likely need to clean that up
> 
> That brown mass is iron oxide (basically rust) as a result of using steel wool in a nitric solution
> 
> Put those filters in a plastic container with a lid on them so they don't dry out (we "may" need to come back to them)
> 
> Put the solutions aside until we are able to discuss this in more detail --- in other words - slow down & in fact stop until "others" have chimed in - instead of just jumping in on the advice of one person
> 
> I say that because "sometimes" there are mis-understandings in what is posted - which may (or not) lead to mistakes made in the advice given - so it is always good to "wait" & hear what others have to say as someone else may catch the mis-understanding & correct it
> 
> I believe that is the situation here
> 
> Steel wool does not work well in a nitric solution (which is what you have) & we are now seeing the results of that
> 
> Steel wool is better suited with HCl solutions
> 
> So Geo did not give bad advice - I "think" he just mis-understood your situation --- waiting for "others" to chime in "may" have avoided the mess(es) you have now created
> 
> Trust me - I to sometime mis-understand what I read - post a reply - & then someone else has to correct me
> 
> My point being - as someone still learning - slow down & wait for others to chime in so that discussions are more complete - instead of just jumping in on the advice of "one" post
> 
> To be continued (all I have time for today)
> 
> Kurt


Hi Kurt !
Yes, Sir ! I sit still in the boat and await further instructions. 
- I do have some other mass/fluids in jars/bottles which needs to be "rescued" later on. My thinking is that Nitric acid can do wonders with them all (going back to "zero"). But lets try to get something positive out first (and secure the method to use).
Br - Lars


----------



## orvi

jphayesjr said:


> During the 1980s and 1990s, Rh was often not even refined out of other PGMs, or gold or silver, it was a cheaper substitute for PT/Pd, it's only large scale commercial use was anti-corrosive plating on silver, especially jewelry.


Depend on where the actual Rh was intended to be used in the mixture. Plating some PGM alloy with Rh in it... I don´t know if it would go as intended. Even in very old appliances (I am used to Soviet manufactured stuff here), all PGMs are refined, palladium contain no Rh when it comes to plating and contact points in relays etc. Only place where I found Rh in old stuff are magnetic contacts, where tip of the pin is Rh plated. And that rhodium is clean, no Pt or Pd, even Ir in it. And we all know that Soviet technology weren´t most efficient and productive. If it was feasible, they would plate mixtures everywhere  

From people here on the forum, and also from my experience, I have never heard of other noble metals present in MLCCs (any types, any time period) than Pd, Pt and Ag. So I will be extra cautious.


----------



## orvi

You created some unhealthy portion of iron oxohydroxide. Impossible to filter, or work with in the sane way. Iron sludge always came out when pH rise above 4 (?? - not certain about number, but it is in close proximity, somebody correct me if im wrong). Precipitate of FeO(OH).xH2O dissolve relatively OK in concentrated HCL. But before doing this discuss it here, as you do not make another stepback.


----------



## kurtak

Sorry but no time to post anything today

Will "try" again" tomorrow

Kurt


----------



## Lars100

kurtak said:


> Sorry but no time to post anything today
> 
> Will "try" again" tomorrow
> 
> Kurt


Hi Kurt !
No problem. I wont do anything this weekend any way.
- And the test with steel wool is no big issue. I used about 3.5dl for this experiment. We still got 12L to work with 
Br Lars


----------



## kurtak

Lars100 said:


> We still got 12L to work with


OK - I am going to "try" to help you out here - BUT - with that said - you have to agree that you are going to slow down & wait for discussion to be complete &/or follow my instructions exactly 

In other words - no more just jumping in on the advice of anyone &/or everyone --- that is what got you in trouble with the steel wool thing

To clarify - there are most certainly others here that can help you - BUT - because you are new to this you really need to follow the lead of one experienced refiner - it doesn't need to be me - it can be any - one - of our well respected refiner's on this forum --- or as the old saying(s) go --- too many cooks spoil the broth or too many cooks in the kitchen spoil the pot - meaning that a plan or project fails because there are too many people working on it at the same time

So - if you want my help - do you agree to follow my lead ?

if so - *this is going to take some time* as we will be doing things (questions & answers) *one at a time* (to insure I understand your situation) & then move forward with recovery *one step at a time*

Do you agree ?

Kurt


----------



## Lars100

Hi Kurt !
Yes, thanks. That suits me just fine ! One step at a time !
Remember that I´m not chemist so You will need to have patience with me (and my equipment -which is not a chemistry lab).
Looking forward to hear how You want me to proceed !
Br Lars


----------



## kurtak

Lars100 said:


> Yes, thanks. That suits me just fine ! One step at a time !


OK - Then the first step(s) is going to be me asking some questions so I can "fully" understand your situation

First - you said ----------



Lars100 said:


> We still got 12L to work with


If I understand right - you got to that 12 liters by doing "several" small batches - is that right ?

If so - how many batches ?

Did you keep each batch separate ?

If kept separate - (about) how much solution from each batch ?

In your OP (first post) you said --------


Lars100 said:


> All,
> I managed to get together quite a pile of MLCC's which are of 2005 or older... Im far from a chemist but have been working with electronics for many years. Got on the track with Palladium when I learned about all the cathalyst´s being stolen from cars and realized that I had these MLCC´s.
> So my goal is to extract as much Palladium and Silver as I can.
> Started watching videos on YouTube how to do this refining and brought together necessary acids (so far...). *Placed the MLCC´s in pet bottles with about 15% HCL to get rid of the tin* (and perhaps outside nickel). Believe I was pretty succesful as I ended up (after about a week) with a purple transparent liquor with grey mass in the bottom (tin ?).
> *Out with the MLCC's and let them just dry up for a while.* *Put the purple liquid aside.
> Bought two mixers with extra blades and grinded the MLCC's to dust (almost). Then into new pet bottles and added concentrated Nitric acid*. Red smoke and red fluid. The mass changed color into greenish/grey.
> *Let it stand for about a week (shaking every day). Out of the bottles and filtered. I have saved the grey green mass in the filters (dont want to throw away...yet).
> The components (whats left of them) into a plastic tray for keeping.
> The filtered fluid is black/green and fairly transparent.
> Added concentrated HCL and the fluid changed color to dark red and in the bottom a separated beige/red mass appeared (silver ?).*


Per the things I highlighted in bold print - that was your "first" batch - is that the "same" process you used on ALL other batches to get to the 12 liters of solution you currently have ?

That includes the step of adding the HCl to "each" batch after the nitic leaching ? --- or did you do that step to only some of the batches ?

In your first post you also said ---------



Lars100 said:


> I have taken some other measures from here but it doesnt seem right.
> For ex. adding sodium and formic acid to the dark red fluid...and heat to about 80C. If I filter that potion and heat again it will only become a black mass.
> If I pore Nitric Acid in that black mass then it melts into a orange/brown tranparent fluid (which in a way must be right but only takes me backwards...) !


Is that the one & only time you did that ?

Or have you done this with some &/or all the 12 liters we still have ?

To be clear - right now I am only interested in the 12 liters we still have - & if (at this point) it has all gone through the same process - or - if different things have been done with different batches

Right now I don't need details on each batch - just need to know if all the batch have been put through the same process & to the same point - or - if different batches have had different thing done to them

Kurt


----------



## Lars100

Hi Kurt !
Several questions...let me try to address them:
*1.* We started out ripping the MLCC´s from their paper rolls...some 30kg...took a while  The MLCC+s were all from 2005 or older. Some were magnetic and some weren´t. We believed that most magnetic was from the outer electrodes which we were going to wash away. So basically we mixed all the MLCC´s in a big jar.
*2.* Then we thought that putting about 7-800gram in a 2 liter PET-bottle was a bright idea. We drowned the MLCC´s in 15% HCL for at least a week (two sometimes). In most cases the fluid turned purple after a little while. In a few cases the fluid turned green (and it seemes like the green is dominant over the purple).
We filtered out the fluid and have kept it but Im not sure why...I don´t believe this fluid (purple of green) contain anything else then lead, tin and maybe some nickel.
*3.* After that we throw together all the MLCC´s in a big jar again and then we took little by little and grinded them in two fruit mixers. I bought some extra blades direct from China (some 30pcs as we destroyed about one blade per kg MLCC).
*4.* After grinding we put back, again, some 7-800g in new 2 liter pet bottles and addes some 4-5dl Nitric acid. 
As You can imagine it was a bit of a dirty story...with boiling, heat and smoke...(we let them boil for themselves...). 
The MLCC´s stayed in the soup for just a week and then we filtered them out. 
We have kept what remains of the MLCC´s in plastic jars with lids on as I think there are more to get from them. Today I believe that the 4-5dl of concentrated Nitric acid should have been more...buy I don´t know...as for now.
*5.* We poured the fluids together (again in 2L pet bottles) and then added some 3 dl concentrated HCL to each bottle. The given "recipe" (from point 1) was given to us on You tube. And after about 24 hours we could see "the silver" come together in the bottom of the bottles. Everything going as planned so far !
We separated "the silver" purely by decanting the fluids from eachother. We got "the silver" in a big glass jar (and haven´t really worked with it...we have done some tests of which we can talk later).
*6.* We continued with "the recipe" and started to add Sodium carbonate in some of the fluid and heating to 80C.
Everything looked fine to begin with but as we started to "boil down" the fluid we just got a black mass (see earlier pictures) while the original on Youtube got a transparent, water clear solution with pd bits floating around in it...just to filter out...
I think we used about two liters trying this method before we stopped.
*7. *Thats when I Iearned about this Forum...and the Steel wool. For this test we used about 3-4dl of the fluid.
*8.* Now we got about 12 liter of the basic Nitric/HCL fluid remaining to work with.

- We can forget about the "steel wool mass". It is very little anyway. More interesting with the "sodium carbonate mass". There must be some 2kg of that one and it´s easy to disolve in Nitric acid (turning orange/brown). But we can go for that one later...

Hope the above can be of guidance and I look forward the hear Your thinking about it all !

- If something sounds stupid then it´s probably because my english is poor. Please excuse me for such errors.

Br - Lars


----------



## Lars100

kurtak said:


> OK - Then the first step(s) is going to be me asking some questions so I can "fully" understand your situation
> 
> First - you said ----------
> 
> 
> If I understand right - you got to that 12 liters by doing "several" small batches - is that right ?
> 
> If so - how many batches ?
> 
> Did you keep each batch separate ?
> 
> If kept separate - (about) how much solution from each batch ?
> 
> In your OP (first post) you said --------
> 
> Per the things I highlighted in bold print - that was your "first" batch - is that the "same" process you used on ALL other batches to get to the 12 liters of solution you currently have ?
> 
> That includes the step of adding the HCl to "each" batch after the nitic leaching ? --- or did you do that step to only some of the batches ?
> 
> In your first post you also said ---------
> 
> 
> Is that the one & only time you did that ?
> 
> Or have you done this with some &/or all the 12 liters we still have ?
> 
> To be clear - right now I am only interested in the 12 liters we still have - & if (at this point) it has all gone through the same process - or - if different things have been done with different batches
> 
> Right now I don't need details on each batch - just need to know if all the batch have been put through the same process & to the same point - or - if different batches have had different thing done to them
> 
> Kurt


Hi Kurt !
Now I answered You in my own comment block (I should have answered You direct). Anyway my answer is published. 
Br - Lars


----------



## kurtak

Hi Lars

Thank you for reply yesterday - this gives me a much better idea of what you have done to get to where you (we) are

I am sending you a PM as I want to discuss some of this in private with you 

Kurt


----------



## jphayesjr

orvi said:


> Depend on where the actual Rh was intended to be used in the mixture. Plating some PGM alloy with Rh in it... I don´t know if it would go as intended. Even in very old appliances (I am used to Soviet manufactured stuff here), all PGMs are refined, palladium contain no Rh when it comes to plating and contact points in relays etc. Only place where I found Rh in old stuff are magnetic contacts, where tip of the pin is Rh plated. And that rhodium is clean, no Pt or Pd, even Ir in it. And we all know that Soviet technology weren´t most efficient and productive. If it was feasible, they would plate mixtures everywhere
> 
> From people here on the forum, and also from my experience, I have never heard of other noble metals present in MLCCs (any types, any time period) than Pd, Pt and Ag. So I will be extra cautious.


Thanks for sharing your experience, Orvi. I accumulated a lot of de-accessioned scrap back in the 70s, 80, 90s from my industrial and govt suction sources. Some, with legitimate help from an uncle who was Chief Metalurgist for GM Electromotive and who was a USAF 2 star, some from friends who worked in Zenith, Motorola, Mallory, Apple, Intel.. One notable exception about items made from Rhodium..."reed relays." In some places, posters call them "quills." Many contain rhodium - silver elements. Some contain silver-palladium/platinum. Some are on PCBs, some are vehicle electrical components, terrestrial, marine, airborne.


----------



## MicheleM

jphayesjr said:


> Thanks for sharing your experience, Orvi. I accumulated a lot of de-accessioned scrap back in the 70s, 80, 90s from my industrial and govt suction sources. Some, with legitimate help from an uncle who was Chief Metalurgist for GM Electromotive and who was a USAF 2 star, some from friends who worked in Zenith, Motorola, Mallory, Apple, Intel.. One notable exception about items made from Rhodium..."reed relays." In some places, posters call them "quills." Many contain rhodium - silver elements. Some contain silver-palladium/platinum. Some are on PCBs, some are vehicle electrical components, terrestrial, marine, airborne.


Please, could you post pictures of these items?


----------



## jphayesjr

MicheleM said:


> Please, could you post pictures of these items?


This weekend


----------



## Geo

jphayesjr said:


> Thanks for sharing your experience, Orvi. I accumulated a lot of de-accessioned scrap back in the 70s, 80, 90s from my industrial and govt suction sources. Some, with legitimate help from an uncle who was Chief Metalurgist for GM Electromotive and who was a USAF 2 star, some from friends who worked in Zenith, Motorola, Mallory, Apple, Intel.. One notable exception about items made from Rhodium..."reed relays." In some places, posters call them "quills." Many contain rhodium - silver elements. Some contain silver-palladium/platinum. Some are on PCBs, some are vehicle electrical components, terrestrial, marine, airborne.


Be very careful handling reed switches. Not all, but enough of the total amount of them contains liquid mercury. They are called "mercury wetted relay" or equivalent warning on the outer case. They are normally encased in a glass tube that is suspended inside a coil of copper on a plastic spool. Inside the tube are two "reeds" extended towards the other from either end surpassing each other by about a quarter of an inch. They are generally in an "open" position while resting. Each reed will have a mirrored appearance that is liquid mercury that is applied to assure connection of the electrodes. If someone was scrap metal intent, the coils would be cut or just broken off of the board and the glass tube shatters and the reed is cut from the board and collected to sell to someone else. You never know. You have to assume that they are all contaminated and work from there.


----------



## MicheleM

you should look carefully before process them, especially the older ones. An example of modern wetted Hg relays;






Mercury Wetted - Standex Electronics







standexelectronics.com





You can find useful info browsing through this link








The Reed Relay Leaders | Reed Relays | Pickering Electronics


Pickering Electronics - Design, manufacture and distribute high quality Reed Relays for Instrumentation, ATE and Semiconductor Test.




www.pickeringrelay.com





Another potentially dangerous element is Ruthenium, a PGM inert metal that react strongly to common bleach. It can form Extremely toxic volatile compounds


----------



## dpgold

Ohiogoldfever said:


> It’s one of the most important things to know before you proceed.
> 
> I use 2 grams of Tin shot in 50ml of Hydrochloric. Filter after dissolving the tin. Works a treat.


how would the solution be affected if the HCL is higher concentration? How would it be different? I used 1 gram if Tin which I scraped away and 5ml of 55percent HCL, should I dilute a bit with water now?


----------



## Yggdrasil

dpgold said:


> how would the solution be affected if the HCL is higher concentration? How would it be different? I used 1 gram if Tin which I scraped away and 5ml of 55percent HCL, should I dilute a bit with water now?


Where did the quote you commented come from?
Some times the things do not make sense, there is an ongoing discussion regarding getting out PM's from MLCCs.
The OP did not know how to make Stannous that is right, but I do not do the relevance to your quote?
Anyway Stannous is not a very picky chemical. 
You put some tin into HCl and let it dissolve as much as it can.
Make sure that there are some extra Tin in there then it will last longer.


----------



## dpgold

Yggdrasil said:


> Where did the quote you commented come from?
> Some times the things do not make sense, there is an ongoing discussion regarding getting out PM's from MLCCs.
> The OP did not know how to make Stannous that is right, but I do not do the relevance to your quote?
> Anyway Stannous is not a very picky chemical.
> You put some tin into HCl and let it dissolve as much as it can.
> Make sure that there are some extra Tin in there then it will last longer.


I put 1g of Tin in 5ml of concentratet (55 percent) HCL, part of the Tin was scraped to dissolve faster and I let some bigger pieces to make it last longer, but I was wondering how much more I can dilute it to make a bit more but still usable. What would be the the rule of thumb when to add Tin or more HCL, I used the proportions I have seen on some videos where the ratio was 2 g Tin to 10 ml of 30 percent HCL. Since I used 55 percent it would seem that I could double the amount of Tin and water to my receipe. The quote was from a discussion about MLCC and testing the PGM content. 
I have about 4kg of MLCC randomly picked from many different boards over time by me and other people magnetic and non magnetic. I was thinking to put it in 30 percent HCL to keep it wet while I still research how I should go about processing them, any idea?


----------



## Yggdrasil

dpgold said:


> I put 1g of Tin in 5ml of concentratet (55 percent) HCL, part of the Tin was scraped to dissolve faster and I let some bigger pieces to make it last longer, but I was wondering how much more I can dilute it to make a bit more but still usable. What would be the the rule of thumb when to add Tin or more HCL, I used the proportions I have seen on some videos where the ratio was 2 g Tin to 10 ml of 30 percent HCL. Since I used 55 percent it would seem that I could double the amount of Tin and water to my receipe. The quote was from a discussion about MLCC and testing the PGM content.
> I have about 4kg of MLCC randomly picked from many different boards over time by me and other people magnetic and non magnetic. I was thinking to put it in 30 percent HCL to keep it wet while I still research how I should go about processing them, any idea?


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.


----------



## 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

Yggdrasil said:


> 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 !!!*


Yggdrasil said:


> 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

Yggdrasil said:


> 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

dpgold said:


> 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

Yggdrasil said:


> 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

Geo said:


> 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

Yggdrasil said:


> 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

MicheleM said:


> 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

MicheleM said:


> 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

galenrog said:


> 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

Geo said:


> 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

Rreyes097 said:


> 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

Yggdrasil said:


> 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.


----------



## Yggdrasil

Rreyes097 said:


> 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.


Well if you have not crushed/milled them into dust, almost all the values are still in there.
And it is time to read Orvis post regarding MLCCs or Kurtaks.

If you just convert to Silver Oxide then you are only half way, you need to convert the Oxide to elemental Silver, before you are finished.

And, Yes the reason to convert to Silver Chloride is to separate the Ag and Pd.
But there is still drag down so one need to clean/wash the Silver Chloride thoroughly.
Then cement out the Pd, this has to be done with aggressive stirring.


----------



## Rreyes097

Yggdrasil said:


> Well if you have not crushed/milled them into dust, almost all the values are still in there.
> And it is time to read Orvis post regarding MLCCs or Kurtaks.
> 
> If you just convert to Silver Oxide then you are only half way, you need to convert the Oxide to elemental Silver, before you are finished.
> 
> And, Yes the reason to convert to Silver Chloride is to separate the Ag and Pd.
> But there is still drag down so one need to clean/wash the Silver Chloride thoroughly.
> Then cement out the Pd, this has to be done with aggressive stirring.


I've been reading all that. And I've also read that crushed or milling isn't necessary. Because the leeching will get to it. But again that's why I'm doing a sample sized run. To learn the proper process for what I'm trying to accomplish. Which is I think just to go for the silver.


----------



## Yggdrasil

Rreyes097 said:


> I've been reading all that. And I've also read that crushed or milling isn't necessary. Because the leeching will get to it. But again that's why I'm doing a sample sized run. To learn the proper process for what I'm trying to accomplish. Which is I think just to go for the silver.


Then you should know that that is completely depending on the composition of the ceramics.
Older will more likely decompose than newer.

So if the MLCCs are whole, they are not leached, if they smoulder to powder they may be. 

And often HCl are better for attacking the Ceramics than Nitric. 

That is the reason Orvi and Kurt are advocating the smelting route.

That route also starts with milling unless you have access to the beauties Orvi showed in his thread


----------



## kurtak

Yggdrasil said:


> So if the MLCCs are whole, they are not leached,


This is absolutely correct

Kurt


----------



## kurtak

Rreyes097 said:


> And I've also read that crushed or milling isn't necessary. Because the leeching will get to it


It may not be necessary to mill them - BUT - if you don't run the leaching process to the point that the ceramic turns to an *ultra fine* ceramic mud you have *NOT* leached all the Ag/Pd out of the ceramic

The Ag/Pd is layered/sintered in the ceramic - as the leaching dissolves the Ag/Pd the ceramic falls apart into ultra fine ceramic particles - leaving you with an ultra fine clay like mud

That mud is *impossible* to filter !!!! 

Therefore you have to wash it with water (to get the leach values out) let the ceramic settle (that can take a day or more) - decant the wash - AND - you have to do multiple washes (3 or MORE) & even then you will never get all the values washed out - there will always be at least "traces" left behind

This results in* VERY *diluted solutions which means *lots *of evaporation is needed before going to recovery of the values from the leach/washing process

At every step of trying to leach MLCCs you are likely to lose at least some values

LOTS of chem waste - time wasted & values lost in leaching MLCCs

Smelting = MUCH less time MUCH less chem waste & MUCH better recovery

For what it is worth

Kurt


----------



## kurtak

Also - for what it is worth - I am still working with Lars100 "trying" to get his values back from the *33kg of MLCCs* he leached --- that has been an on going "daily" project *for 7 months now*

We are now "finally" to a point of working on the recovery of the values from the leach - AND - we have no idea of how much values have been left behind in the ceramic mud &/or other waste

So we will have go back & test/assay all of that to see if it is worth going back to - to chase (because values are always left behind with leaching)

It is one thing to leach 1Kg MLCCs - but 33kg - *what a mess !!!!!!!!!*

if Lars had smelted those MLCCs he (we) would have been 6 months ago - had better recovery - used MUCH less chem - with MUCH less chem waste

The problem --- Lars (before coming to this forum) watched some *"back yard hacks"* leach MLCCs & followed the advice of those "back yard hack" - not realizing (at the time) just *how bad* the advice to leach MLCCs really is

IMO - even small batches should be smelted 

Again - for what it is worth

Kurt


----------



## kurtak

Rreyes097 said:


> But again that's why I'm doing a *sample sized run. To learn the proper process* for what I'm trying to accomplish.



Per the bold print - if you really want to learn the "proper process" - *learn to smelt !!!!!*

Leaching *a small* sample will give you results without to much problem/mess - BUT - that will *most certainly* lead you to believe - cool - now I can move up to leaching *bigger* batches - that will most certainly result in nothing other then *bigger problems/messes*

In other words - leaching (MLCCs) is a case where bigger is *absolutely not better* --- in fact - the bigger you go - *the WORSE it gets !!!! *


Rreyes097 said:


> Which is I think just to go for the silver.



If you are going to go after the values in MLCCs - why in the world you go after "just the silver --- the real value is the Pd 

Current silver value = 68 cents per gram 

Current palladium value = $58.26 per gram

Kurt


----------



## Rreyes097

kurtak said:


> Per the bold print - if you really want to learn the "proper process" - *learn to smelt !!!!!*
> 
> Leaching *a small* sample will give you results without to much problem/mess - BUT - that will *most certainly* lead you to believe - cool - now I can move up to leaching *bigger* batches - that will most certainly result in nothing other then *bigger problems/messes*
> 
> In other words - leaching (MLCCs) is a case where bigger is *absolutely not better* --- in fact - the bigger you go - *the WORSE it gets !!!! *
> 
> 
> If you are going to go after the values in MLCCs - why in the world you go after "just the silver --- the real value is the Pd
> 
> Current silver value = 68 cents per gram
> 
> Current palladium value = $58.26 per gram
> 
> Kurt


Because most of what I'm told I have( magnetic) has or most likely has no palladium. Gave me something to think about there.


----------



## Geo

Converting the silver to silver chloride is not just to chase the silver. It is actually part of the process of chasing the Pd. In a nitrate solution, both silver and Pd are in liquid form. If you cement on copper from here, you will still have silver and palladium mixed. If you add chlorine, the silver will turn into a solid (AgCl2) and will settle out or be filtered leaving palladium in solution effectively separating the two metals. The silver and it's recovery is secondary to the recovery of the Pd.


----------



## Rreyes097

Ok so I'll research smelting. But I'm not sure I have the proper equipment.


----------



## orvi

Rreyes097 said:


> Ok so I'll research smelting. But I'm not sure I have the proper equipment.


Wet-leaching MLCCs is doable, Owltech has great video about it on YouTube. But overall process is far from nice and efficient. And also it is necessary to point out that unless the caps arent from the "good" ceramic material - namely barium titanate ceramics or other favourable types, they doesn´t even disintegrate in acids AT ALL. So nothing is achieved by this step in some cases. 

Most likely, modern types are composites of titanates with alumina or zirconia, some wild niobium additives and other stuff. Acid attacks only leachable parts, leaving ultrafine TiO2, Al2O3 and ZrO2, which aren´t filterable and clog any filter, worse than metastannic acid. And decantation is a process where certain proportion of values is still trapped in the mud. So you need to repeat the process numerous times - insanely increasing volume of the solution = creating buckets and buckets of waste to be dealt with... Not nice.

Question is, do you want to continue with refining in the future ? I mean, serious refining. If your answer is yes, then invest in proper equipment.* As probably all members here know, I am strong advocate for induction furnance*. Small types going up to 7-8kW of real heating power are relatively cheap, selling under 800 bucks on Aliexpress. Despite the fact they are genuinely Chinese machines, they run nicely, and I never had any problem with them (actually we have two, one large 35kW one). And we abused them A LOT.

Practically ALL your casual melting can be done in an induction furnance. It is very energy effective heating device = proportion of heat used vs. necessary to attain the required temperature is very nice, compared to indirect heating techniques like using gas torch or gas furnance.* With induction, your temperature limit is practically sublimation point of carbon = using graphite crucibles allow you to go sanely to like 2000°C. Then it burns too quickly in the air  *

So not only for copper, gold and silver. Palladium and platinum like a piece of cake. Even rhodium is nicely melted, when you insert the magnesia crucible inside the graphite one to prevent carbides formation. I do not say this is proper melting technique for these metals (and for Pd certainly isn´t), but much easier and "better" than bleeding with handheld oxy-acetylene, spitting half of the charge around the melt dish, even if you try to not to.

Think about it and I would suggest to give it a shot. 7kW is a LOT of power to be concentrated to one small crucible, so melting IS FAST. Ordinary melting of silver to 0,5-1kg ingots is done in order of minutes. Consistently, predictably, no metal contamination from the tip of the torch... Quite a lot of advantages


----------



## Rreyes097

orvi said:


> Wet-leaching MLCCs is doable, Owltech has great video about it on YouTube. But overall process is far from nice and efficient. And also it is necessary to point out that unless the caps arent from the "good" ceramic material - namely barium titanate ceramics or other favourable types, they doesn´t even disintegrate in acids AT ALL. So nothing is achieved by this step in some cases.
> 
> Most likely, modern types are composites of titanates with alumina or zirconia, some wild niobium additives and other stuff. Acid attacks only leachable parts, leaving ultrafine TiO2, Al2O3 and ZrO2, which aren´t filterable and clog any filter, worse than metastannic acid. And decantation is a process where certain proportion of values is still trapped in the mud. So you need to repeat the process numerous times - insanely increasing volume of the solution = creating buckets and buckets of waste to be dealt with... Not nice.
> 
> Question is, do you want to continue with refining in the future ? I mean, serious refining. If your answer is yes, then invest in proper equipment.* As probably all members here know, I am strong advocate for induction furnance*. Small types going up to 7-8kW of real heating power are relatively cheap, selling under 800 bucks on Aliexpress. Despite the fact they are genuinely Chinese machines, they run nicely, and I never had any problem with them (actually we have two, one large 35kW one). And we abused them A LOT.
> 
> Practically ALL your casual melting can be done in an induction furnance. It is very energy effective heating device = proportion of heat used vs. necessary to attain the required temperature is very nice, compared to indirect heating techniques like using gas torch or gas furnance.* With induction, your temperature limit is practically sublimation point of carbon = using graphite crucibles allow you to go sanely to like 2000°C. Then it burns too quickly in the air *
> 
> So not only for copper, gold and silver. Palladium and platinum like a piece of cake. Even rhodium is nicely melted, when you insert the magnesia crucible inside the graphite one to prevent carbides formation. I do not say this is proper melting technique for these metals (and for Pd certainly isn´t), but much easier and "better" than bleeding with handheld oxy-acetylene, spitting half of the charge around the melt dish, even if you try to not to.
> 
> Think about it and I would suggest to give it a shot. 7kW is a LOT of power to be concentrated to one small crucible, so melting IS FAST. Ordinary melting of silver to 0,5-1kg ingots is done in order of minutes. Consistently, predictably, no metal contamination from the tip of the torch... Quite a lot of advantages


Wow lots to think about. I do intend to continue refining. And I have invested lots into the hobby. But money is right now so any money I put back into it needs to be made from it. With the mlccs I was just trying to learn the process. And while trying to learn said process I've encountered this ceramic and it's incredible power to lock up the filter.  So I'm seeing the smelting as probably the way to go but now I have to learn and research a whole another aspect of refining. Would a electric furnace be enough? Until I can invest in all the equipment I need?


----------



## orvi

Rreyes097 said:


> Wow lots to think about. I do intend to continue refining. And I have invested lots into the hobby. But money is right now so any money I put back into it needs to be made from it. With the mlccs I was just trying to learn the process. And while trying to learn said process I've encountered this ceramic and it's incredible power to lock up the filter.  So I'm seeing the smelting as probably the way to go but now I have to learn and research a whole another aspect of refining. Would a electric furnace be enough? Until I can invest in all the equipment I need?


Practically speaking, kind of. Electric can´t go to that high temperatures, and past 1300-1400°C, most of the wiring simply erode and brake too quickly. You need to be able to re-wire the furnance, adding cost of the quality wiring, which isn´t cheap. So you will be kind of able to smelt the MLCCs, but not able to eg melt final refined palladium or platinum in it, or pyrometallurgically refine the Pd (which is the easiest way for rough cleaning).


----------



## kurtak

Rreyes097 said:


> Would a electric furnace be enough?



If you are talking about electric furnace like this --------









VEVOR Electric Melting Furnace, 3KG Digital Electric Melting Furnace, 1750W 1150℃/2102 ℉ Gold Smelter Furnace W/ 1KG&3KG Graphite Crucible & Ingot Die for Processing of Melting Gold, Silver, Copper | VEVOR US


Discover VEVOR Electric Melting Furnace, 3KG Digital Electric Melting Furnace, 1750W 1150℃/2102 ℉ Gold Smelter Furnace W/ 1KG&3KG Graphite Crucible & Ingot Die for Processing of Melting Gold, Silver, Copper, Professional Melting Furnace and High-Purity Graphite Crucible at lowest price, 2days...




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*NO !!!* --- they are ok for melting "pure" metals (but even then I do not recommend them - waste of money IMO)

They DO NOT work *at all* for smelting - the FIRST time you have a flux boil over (which *IS* going to happen) it destroys the heating elements

Edit to add; - they get hot enough to melt silver - barely hot enough (though they will) to melt gold - NOT hot enough to melt copper 

If you are going to smelt you need ether a propane fired or induction furnace

Kurt


----------



## orvi

kurtak said:


> If you are talking about electric furnace like this --------
> 
> 
> 
> 
> 
> 
> 
> 
> 
> VEVOR Electric Melting Furnace, 3KG Digital Electric Melting Furnace, 1750W 1150℃/2102 ℉ Gold Smelter Furnace W/ 1KG&3KG Graphite Crucible & Ingot Die for Processing of Melting Gold, Silver, Copper | VEVOR US
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> *NO !!!* --- they are ok for melting "pure" metals (but even then I do not recommend them - waste of money IMO)
> 
> They DO NOT work *at all* for smelting - the FIRST time you have a flux boil over (which *IS* going to happen) it destroys the heating elements
> 
> Edit to add; - they get hot enough to melt silver - barely hot enough (though they will) to melt gold - NOT hot enough to melt copper
> 
> If you are going to smelt you need ether a propane fired or induction furnace
> 
> Kurt


As long as you want to obviate the correct solution to the problem, you will find yourself in even bigger mess  correct  greatly apply to the field of refining.

Induction has also one advantage - whole machine is practically separated from the place where you melt, coil being separated from the whole machine = you can nicely insulate the machine box from the heat produced = for sane power output rating, it never suffer from heat generated during melting or smelting. Folded aluminium foil mostly being completely enough to do the job perfectly. 

If some boil-over DO occur in induction, you will likely just melt your insulation mineral wool with molten flux. In extreme case coil could possibly be damaged. But anyway, that is few bucks for new copper pipe  nothing major. And by the way, it never occured to me to damage coil in a way I would need to replace it. Some coils we use are in service for more than 4-5 years - working hard over those years


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## Rreyes097

orvi said:


> Practically speaking, kind of. Electric can´t go to that high temperatures, and past 1300-1400°C, most of the wiring simply erode and brake too quickly. You need to be able to re-wire the furnance, adding cost of the quality wiring, which isn´t cheap. So you will be kind of able to smelt the MLCCs, but not able to eg melt final refined palladium or platinum in it, or pyrometallurgically refine the Pd (which is the easiest way for rough cleaning).


Mine goes to 2000°Fv how much is that in centigrade? Either way it sounds like it's not hot enough.


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## orvi

Rreyes097 said:


> Mine goes to 2000°Fv how much is that in centigrade? Either way it sounds like it's not hot enough.


Yup, you are right. Barely enough to melt gold. 2000F is around 1090 °C. You need to go more to the range of 1400-1500°C. That is around 2500F and more. Electric tabletop furnance does not gonna make it


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## Rreyes097

orvi said:


> As long as you want to obviate the correct solution to the problem, you will find yourself in even bigger mess  correct  greatly apply to the field of refining.
> 
> Induction has also one advantage - whole machine is practically separated from the place where you melt, coil being separated from the whole machine = you can nicely insulate the machine box from the heat produced = for sane power output rating, it never suffer from heat generated during melting or smelting. Folded aluminium foil mostly being completely enough to do the job perfectly.
> 
> If some boil-over DO occur in induction, you will likely just melt your insulation mineral wool with molten flux. In extreme case coil could possibly be damaged. But anyway, that is few bucks for new copper pipe  nothing major. And by the way, it never occured to me to damage coil in a way I would need to replace it. Some coils we use are in service for more than 4-5 years - working hard over those years


My electric furnace burnt it's heating element within the first 2 to 3 months. So yes I know first hand that they are cheap.


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## Rreyes097

orvi said:


> Yup, you are right. Barely enough to melt gold. 2000F is around 1090 °C. You need to go more to the range of 1400-1500°C. That is around 2500F and more. Electric tabletop furnance does not gonna make it


Yeah I realized that when I went to melt some gold and it only got hot enough by adding another torch. but I'm not it about to buy a new one right now. I just lost my job because of not enough work to be had. So I got laid off.


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## orvi

Rreyes097 said:


> My electric furnace burnt it's heating element within the first 2 to 3 months. So yes I know first hand that they are cheap.


That is why I am advocating for permanent solution to much of the pyro-work. Reliable, robust, effective and able to melt anything you will likely encounter, even vaporize carbon if you feel like it


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## GoIdman

Rreyes097 said:


> My electric furnace burnt it's heating element within the first 2 to 3 months. So yes I know first hand that they are cheap.


Try to find a used calcination furnace used in dental labs something like in the link. https://www.linn-high-therm.de/products/details/lm-model.html .. The heating wire can be exchanged if broken, good quality kanthal wire can be bought from aliexpress for like 2-3 usd per 3kW. It lasts forever and goes up to 1350 C.

I rebuilt mine , i have 2 spare wires if it burns, changing the wire is max 30min. 

If the funace is not operational you may even get it for free. Try dental labs if they have broken furnaces, you can refurb one yourself, its straightforward.

Those cheap chinese furnaces eat crucibles and heating elements like crazy, not economical at all.

I`ve never attempted smelting since i am not familiar with that process, but i presume i could use my furnace for that purpose too.

Be safe

Pete


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## kurtak

GoIdman said:


> I`ve never attempted smelting since i am not familiar with that process, but i presume i could use my furnace for that purpose too.



If the heating elements in the (electric) furnace are exposed they (the furnace) is not a good option for smelting in

The fumes generated (which are high temp fumes & corrosive) during smelting will destroy the elements in "relatively" short time - so you will be replacing the elements "relatively" often --- relatively = more often when smelting compared to when just melting pure metals

The high temp corrosive fumes generated during smelting come primarily (but not exclusively) from the flux --- especially if oxidizing flux such a potassium nitrate (as *one* example) are used

If the heating elements go around all side of the furnace (including the floor) *the first time* you have a flux "boil over" (which *IS* going to happen) it is going to destroy the elements

Not saying an electric furnace can't be used for smelting - they just are not a good option for smelting

Kurt


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## Alondro

orvi said:


> That is why I am advocating for permanent solution to much of the pyro-work. Reliable, robust, effective and able to melt anything you will likely encounter, even vaporize carbon if you feel like it


I built a wood-fired furnace long ago with just scrap brick and cinderblock. Only used about 12 fire bricks for the bottom and two sides. Since it was constructed like a chimney, with steel rebar between one lower layer of brick to elevate the fire and allow airflow to move swiftly through it, I could get that thing just hot enough to melt copper. But I needed to have a wheelbarrow full of very dry wood ready each time, and it burned it all in about an hour. With a cast iron crucible made from pipe and plugged at the bottom with refractory cement, it was fantastic for processing aluminum. I only tried to melt copper in the crucible once, but I didn't have enough good hardwood wood to hold temperature long enough to melt more than a fraction of the copper in the crucible. Pine wood doesn't burn long enough or hot enough. 

I'll be building my Model 2 furnace of that type this spring, adapting what I learned from the limits of the first one. I believe I can hit 2200F with it and hold it there with enough hardwood. I'm also going to adapt it to use coal. I have a supply of old weathered coal from a long-abandoned rail track behind my development. The small chunks of PA-origin anthracite coal have been washed in rain and snow for 70 years, and now burns exceedingly clean, with no smoke at all. I'll be curious to see how high the temp will go with that.


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## orvi

Alondro said:


> I built a wood-fired furnace long ago with just scrap brick and cinderblock. Only used about 12 fire bricks for the bottom and two sides. Since it was constructed like a chimney, with steel rebar between one lower layer of brick to elevate the fire and allow airflow to move swiftly through it, I could get that thing just hot enough to melt copper. But I needed to have a wheelbarrow full of very dry wood ready each time, and it burned it all in about an hour. With a cast iron crucible made from pipe and plugged at the bottom with refractory cement, it was fantastic for processing aluminum. I only tried to melt copper in the crucible once, but I didn't have enough good hardwood wood to hold temperature long enough to melt more than a fraction of the copper in the crucible. Pine wood doesn't burn long enough or hot enough.
> 
> I'll be building my Model 2 furnace of that type this spring, adapting what I learned from the limits of the first one. I believe I can hit 2200F with it and hold it there with enough hardwood. I'm also going to adapt it to use coal. I have a supply of old weathered coal from a long-abandoned rail track behind my development. The small chunks of PA-origin anthracite coal have been washed in rain and snow for 70 years, and now burns exceedingly clean, with no smoke at all. I'll be curious to see how high the temp will go with that.


I would definitely stick to the whatever coal rather than wood. Much better energy density. I had charcoal powered small furnance back in my teenage years - which was allright to melt aluminium, but copper was too difficult. But with better insulation, I would melt copper easily in it.

But from practical point of view, this is completely out of scope for me now. It is always such a chore to get it hot in the first place, burn quantities of coal to get to like 1250°C to start doing something useful with it.
One of the best solid fuels is coke. Hard to ignite, but then when it kicks, that´s whole another story. With improper control of the blowing air, I once started to melt firebricks on the bottom of the furnance  
All solid fuel furnances, altough DIY made are very sloppy for fine melting works, flying ashes or another things can mess up whole smelt, not speaking of inability to access temps for PGM working.


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## GoIdman

kurtak said:


> If the heating elements in the (electric) furnace are exposed they (the furnace) is not a good option for smelting in
> 
> The fumes generated (which are high temp fumes & corrosive) during smelting will destroy the elements in "relatively" short time - so you will be replacing the elements "relatively" often --- relatively = more often when smelting compared to when just melting pure metals
> 
> The high temp corrosive fumes generated during smelting come primarily (but not exclusively) from the flux --- especially if oxidizing flux such a potassium nitrate (as *one* example) are used
> 
> If the heating elements go around all side of the furnace (including the floor) *the first time* you have a flux "boil over" (which *IS* going to happen) it is going to destroy the elements
> 
> Not saying an electric furnace can't be used for smelting - they just are not a good option for smelting
> 
> Kurt


Thank you for the valuable info and insight, i will probably bild a gas operating furnace if i want to attempt smelting, the large crucibles are very expensive in my area.
Allthough my furnace has an evacuation pipe in the back, a 1 inch diameter with fan, i presume that is not enough for the large amount of toxic fumes.

Maybe i bild a gas operated furnace. 

Pete


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## Rreyes097

kurtak said:


> It may not be necessary to mill them - BUT - if you don't run the leaching process to the point that the ceramic turns to an *ultra fine* ceramic mud you have *NOT* leached all the Ag/Pd out of the ceramic
> 
> The Ag/Pd is layered/sintered in the ceramic - as the leaching dissolves the Ag/Pd the ceramic falls apart into ultra fine ceramic particles - leaving you with an ultra fine clay like mud
> 
> That mud is *impossible* to filter !!!!
> 
> Therefore you have to wash it with water (to get the leach values out) let the ceramic settle (that can take a day or more) - decant the wash - AND - you have to do multiple washes (3 or MORE) & even then you will never get all the values washed out - there will always be at least "traces" left behind
> 
> This results in* VERY *diluted solutions which means *lots *of evaporation is needed before going to recovery of the values from the leach/washing process
> 
> At every step of trying to leach MLCCs you are likely to lose at least some values
> 
> LOTS of chem waste - time wasted & values lost in leaching MLCCs
> 
> Smelting = MUCH less time MUCH less chem waste & MUCH better recovery
> 
> For what it is worth
> 
> Kurt


Thanks guys. So just with this 20 gram batch I could see how difficult that ceramic was going to be. Because although I only had to deal with a little amount, it was plenty for it to stop up my filter. So I've been trying to research on the forum smelting but I haven't seen anything thus far for what I need. Which is day one, base knowledge first day on the job sort of stuff. I'm sure I know some things but I'd like to know everything I can before trying it. Anybody have any links that they know of?


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## Yggdrasil

Rreyes097 said:


> Thanks guys. So just with this 20 gram batch I could see how difficult that ceramic was going to be. Because although I only had to deal with a little amount, it was plenty for it to stop up my filter. So I've been trying to research on the forum smelting but I haven't seen anything thus far for what I need. Which is day one, base knowledge first day on the job sort of stuff. I'm sure I know some things but I'd like to know everything I can before trying it. Anybody have any links that they know of?


The search function is your friend.
Search and read, the threads that have interesting stuff in them, has to be read completely. There is literally nuggets in here, you just have to find them.
As in real life, they don’t necessarily come easy


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## Rreyes097

So I filtered the 20g mlccs after letting it sit in nitric acid diluted with distilled water for 4 days. After many rinses with distilled water. I then evaporated some so it wasn't so much rinse liquid. I may have lost some values? I'm not sure. But then I used HCl to push out the silver chloride. I converted it and so here is a picture of it. Not sure how much it weighs but by the the looks of it not very much at all. But I don't myself going that route again with even materials. Before I dropped silver I tested it with stannous and it came up negative for pd and gold. So I got whatever silver I could since the mlccs weren't milled or even crushed to be honest. So I'll clean up that little bit of silver and put it with my other recovered silver. Then l suppose I'll go play with my best friend the "search button" thanks y'all for the input. I've got learning to do.


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## Yggdrasil

Rreyes097 said:


> So I filtered the 20g mlccs after letting it sit in nitric acid diluted with distilled water for 4 days. After many rinses with distilled water. I then evaporated some so it wasn't so much rinse liquid. I may have lost some values? I'm not sure. But then I used HCl to push out the silver chloride. I converted it and so here is a picture of it. Not sure how much it weighs but by the the looks of it not very much at all. But I don't myself going that route again with even materials. Before I dropped silver I tested it with stannous and it came up negative for pd and gold. So I got whatever silver I could since the mlccs weren't milled or even crushed to be honest. So I'll clean up that little bit of silver and put it with my other recovered silver. Then l suppose I'll go play with my best friend the "search button" thanks y'all for the input. I've got learning to do.


How did you convert it?


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## Rreyes097

Sodium hydroxide and sugar


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## Yggdrasil

Rreyes097 said:


> Sodium hydroxide and sugar


Then I think there might be something off with your process.
It is supposed to be a light grey heavy powder, not black.
Is it a light issue maybe?


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## Rreyes097

Well it's pretty dark but I guess u could call it dark dark brown but I'm not sure. Could I have not put enough in or either? Well I'll clean it up and maybe it will change to the proper color. Sorry about that


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## Yggdrasil

Rreyes097 said:


> Well it's pretty dark but I guess u could call it dark dark brown but I'm not sure. Could I have not put enough in or either? Well I'll clean it up and maybe it willúmh will it 4u7ll


Can you try again, can’t understand the last part.


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## Yggdrasil

Rreyes097 said:


> Well it's pretty dark but I guess u could call it dark dark brown but I'm not sure. Could I have not put enough in or either? Well I'll clean it up and maybe it willúmh will it 4u7ll


Anyway.
Can you describe in detail what you did and what happened?
There is definitely something off.
Edit for spelling


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## eaglekeeper

Unless the lighting is bad, I would say something is off. Did you use plain old table sugar or something else?. As Yggdrasil mentioned, It should be a bright gray/silvery color.


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## Rreyes097

Yggdrasil said:


> Anyway.
> Can you describe in datail what you did and what happened?
> There us definitely something off.


All I did was follow the people name owl something. Owltech I think they are called. I simply put on my hot plate with magnetic mlccs and heated it up. While magnetic stirrer. Added about 2 maybe 3 tbsp sodium hydroxide. Until everything went from the to pretty much the same color it is now. Then I added regular sugar. This is where I wasn't sure how much sugar.


eaglekeeper said:


> Unless the lighting is bad, I would say something is off. Did you use plain old table sugar or something else?. As Yggdrasil mentioned, It should be a bright gray/silvery color.


Just regular sugar.


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## kurtak

It is black/brown because it is still silver oxide


Rreyes097 said:


> Just regular sugar.


You "should" use Kero syrup (corn syrup) regular sugar will work but corn syrup works better

That is because corn syrup is a reducing sugar (so better reduces silver oxide to actual silver) whereas regular sugar is not a reducing sugar

Also - though not absolutely necessary - you are better served if you wash all the hydroxide out of the AgO before using the sugar to convert the AgO to Ag

Kurt


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## Rreyes097

kurtak said:


> It is black/brown because it is still silver oxide
> 
> You "should" use Kero syrup (corn syrup) regular sugar will work but corn syrup works better
> 
> That is because corn syrup is a reducing sugar (so better reduces silver oxide to actual silver) whereas regular sugar is not a reducing sugar
> 
> Also - though not absolutely necessary - you are better served if you wash all the hydroxide out of the AgO before using the sugar to convert the AgO to Ag
> 
> Kurt


Oh thanks Kurt. I forgot about the washing after the sodium hydroxide. So what should I do now? More sugar? And next time I'll try and pick some of that kero syrup.


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## Yggdrasil

Rreyes097 said:


> All I did was follow the people name owl something. Owltech I think they are called. I simply put on my hot plate with magnetic mlccs and heated it up. While magnetic stirrer. Added about 2 maybe 3 tbsp sodium hydroxide. Until everything went from the to pretty much the same color it is now. Then I added regular sugar. This is where I wasn't sure how much sugar.
> 
> Just regular sugar.


You confuse me. Did you try that procedure with the MLCCs directly?

If that is the case.
You REALLY need to study until you understand.
That precedure is for converting clean Silver Chloride to Silver Oxide and then to Silver.

So please do a step by step of what you did and what happened.


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## Rreyes097

Yggdrasil said:


> You confuse me. Did you try that procedure with the MLCCs directly?
> 
> If that is the case.
> You REALLY need to study until you understand.
> That precedure is for converting clean Silver Chloride to Silver Oxide and then to Silver.
> 
> So please do a step by step of what you did and what happened.


What do you mean directly? Did i have the mlccs in there while I added the sodium hydroxide and then the sugar. So if you are asking if the mlccs were in the beaker will add that stuff then the answer is no. 
After I put the mlccs into dilute nitric I then filtered out the mlccs. And many rinses with distilled water. Next I put the beaker back on the hot plate. Without lid, I tried to evaporate much of the liquid. Then i added sodium hydroxide and used my magnetic stirrer until all of the white chloride turned dark to even black. Next I added the sugar, regular sugar ( which I'm your I should used kero syrup and also should have rinsed that sugar before adding the sugar) so after adding that sugar I kept it in hot plate until it all looked dark and uniform color. Did I mess up? I guess I should have rinsed before sugar but all in all I followed instructions instructions according to my research.


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## Yggdrasil

Rreyes097 said:


> What do you mean directly? Did i have the mlccs in there while I added the sodium hydroxide and then the sugar. So if you are asking if the mlccs were in the beaker will add that stuff then the answer is no.
> After I put the mlccs into dilute nitric I then filtered out the mlccs. And many rinses with distilled water. Next I put the beaker back on the hot plate. Without lid, I tried to evaporate much of the liquid. Then i added sodium hydroxide and used my magnetic stirrer until all of the white chloride turned dark to even black. Next I added the sugar, regular sugar ( which I'm your I should used kero syrup and also should have rinsed that sugar before adding the sugar) so after adding that sugar I kept it in hot plate until it all looked dark and uniform color. Did I mess up? I guess I should have rinsed before sugar but all in all I followed instructions instructions according to my research.


That is great, because in your post to which I replied you seemed to just add NaOH to the MLCCs.
Read it again and you will see.

But as Kurt said you need to wash it properly after.
But for 20grams of MLCCs there should just be minute amount of Silver.
Maybe in best case 2 grams, but since these are magnetic I would guess less than one.


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## Rreyes097

Yggdrasil said:


> That is great, because in your post to which I replied you seemed to just add NaOH to the MLCCs.
> Read it again and you will see.
> 
> But as Kurt said you need to wash it properly after.
> But for 20grams of MLCCs there should just be minute amount of Silver.
> Maybe in best case 2 grams, but since these are magnetic I would guess less than one.


It looks about a gram in there maybe a little less maybe little more.


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## Rreyes097

"So I filtered the 20g mlccs after letting it sit in nitric acid diluted with distilled water for 4 days. After many rinses with distilled water. I then evaporated some so it wasn't so much rinse liquid. I may have lost some values?" This is what I posted. I'm not sure where I confused you but it says right here that I used nitric acid with distilled water. 

But either way. My next step is to maybe grind up the 20g of mlccs and put bank into nitric acid and distilled water. To see if I can get any silver left over because since I didn't mill them out grind them I may have left some silver behind. The stannous never showed any positive findings for Pd so I'm going to just double check it. While I do that I'll be looking for information on smelting. And also create a design to build a furnace so I can do more incineration on mlccs and IC chips. And wherever else may be needing. Sound good?


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## Yggdrasil

I asked you to give a detailed explanation and this is what you gave us:


We have no means to know what you have been doing in the mean time as this rolls ahead.
When we ask for detailed it needs to be detailed for a reason.


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## Rreyes097

Yggdrasil said:


> I asked you to give a detailed explanation and this is what you gave us:
> View attachment 53323
> 
> We have no means to know what you have been doing in the mean time as this rolls ahead.
> When we ask for detailed it needs to be detailed for a reason.


Of course. I'm not saying anything to cause offense. I just didn't understand where I was unclear in my description of my steps up to this point. So thanks for your help, everytime anyone responds I am truly grateful.


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## Rreyes097

By chance would molasses work instead of sugar? Because I don't have Karo but will get it if that's the best option. I'm just wondering.


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## orvi

Rreyes097 said:


> By chance would molasses work instead of sugar? Because I don't have Karo but will get it if that's the best option. I'm just wondering.


If it isn´t hot, reduction is sluggish or even non-proceeding. Regular sugar is more than good for this. Just need to be still very basic and HOT. At least 90°C, and add the sugar in small increments with stirring, as it will quickly heat up and eventually can boil.

With ozt or more batches, I always advise to use the thermometer sticked into the reaction for measuring the temperature. Heat past 95°C preferrably, then began additions of sugar proportional to the silver. It takes just a spoon or two to fully reduce ozt of silver. Temp rise isn´t sudden, it goes slowly and then shoot up quickly. Be prepared. 

Never add more if the temperature isn´t higher than 90 °C, because you do not know if there is some unreacted sugar waiting for it´s chance to create boilover. Also, never add more unless you see sharply that temperature raised and then started to DECLINE. Past 113°C, you can experience mild bubbling and past 115°C it isn´t guaranteed it won´t splash the hydroxide all over you 

Hot lye in the eye isn´t fun. I experienced it. Despite having face shield


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## Rreyes097

Ohiogoldfever said:


> The difference in testing style are purely preference.
> 
> Use filter paper, or a testing dish, spoon..... All you’re doing is maintaining a controlled space for your sample.


I use a qtip


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