Refining MLCC´s for Palladium and Silver !
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Is that what you got from my reply?
I suggest you read it again.
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 !
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 !
Ohiogoldfever
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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.
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.
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 !
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 !
Ohiogoldfever
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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.
I use 2 grams of Tin shot in 50ml of Hydrochloric. Filter after dissolving the tin. Works a treat.
Ohiogoldfever
Well-known member
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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.
Use filter paper, or a testing dish, spoon..... All you’re doing is maintaining a controlled space for your sample.
gldfever87
MDG Refining LLC
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... 
Geo
Well-known member
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.
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.
Geo
Well-known member
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.
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...
kurtak
Well-known member
Per the bold print (in above quote) - NO
Read BOTH of these threads & read them COMPLETELY
https://goldrefiningforum.com/threads/when-in-doubt-cement-it-out.30236/#post-324900
https://goldrefiningforum.com/threads/fuzz-button-interconnects-need-some-advice.22203/#p232030
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)...
kurtak
Well-known member
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 !
MicheleM
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OT for @Geo :do you know this YT channel? your video inside : https://m.youtube.com/user/propeter13
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.
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.
Geo
Well-known member
I do not.
Geo
Well-known member
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.
