# sodium chlorate - palladium process



## Rotz (Mar 1, 2021)

Hello GRF, 

I took black powder from my stock pot, saturated with copper. Then with AR I took the gold. When I see dark brown color at stannous. Then add until saturated with ammonium chloride, nothing show up. Then I add sodium chlorate, greenish yellow salt show up. photo is below. Stannous give negative.

Normally palladium salt looks red but this is yellow. Then I researched the forum. At past, HaroldV had been expressed with photo. it is yellow with sodium chlorate. Then He told if you apply with ammonia step it will be red. Must I apply ammonia step or can I roast directly.


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## Martijn (Mar 1, 2021)

Pd expected solution? Gloves? :!: :!: 

Hi Rotz, what was saturated with copper? The solution or the black powder?
If you have a lot of copper in your pregnant solution the copper can give a false positive with stannous. 
Dilute the drop you test to see the color better.
Martijn.


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## Rotz (Mar 1, 2021)

Hello Marjtin,

I just took a photo so had not gloves. I put copper to my stock pot. Then I took a lot of black powder deep. Dissolve it with hcl and peroxide. When I check stannous I saw purple. Then I precipitate the gold with copperas. Then I saw brown with stannous. It is a like caramel color. Then I added ammonium chloride. Nothing happen and stannous show still same color. I add a lot of when the solution about 40 C. Nothing show up. Stannous still same. So I add sodium chlorate for Cl supplier. Then this material show up. Stannous been negative. I couldnt tell well explained sorry about that. Sometimes I think you know this step and I dont tell all of detail. It is because of my excited. So I tried to see the stannous test again I dissolve a little bit this yellowish sediment in hcl. It didnt give positive result. It is looks like palladium salt but everybody have red I have yellowish. Which process I need to continue. Than you for helping.


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## Rotz (Mar 1, 2021)

By the way I know false positive result. It is not that.


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## Rotz (Mar 1, 2021)

Martijn said:


> Pd expected solution? Gloves? :!: :!:
> 
> Hi Rotz, what was saturated with copper? The solution or the black powder?
> If you have a lot of copper in your pregnant solution the copper can give a false positive with stannous.
> ...



I saw this post today. It is quite similar color. Should I apply ammonia and hcl to make red ?


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## Rotz (Mar 2, 2021)

This is the color of stannous before it precipitated.


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## Martijn (Mar 2, 2021)

Sorry, that was all I could contribute. No practical experience with Pd. You need more knowledgeable members to respond here. 
good luck


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## Rotz (Mar 2, 2021)

Thank you I hope I can refine


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## Yggdrasil (Mar 2, 2021)

The stannous looks like "false positive" to me.
In my humble not too experienced world I would guess copper or something like that.
You can see the "clear" liquid with the brown precipitate in it.


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## Rotz (Mar 2, 2021)

I don't think false positive. I tried my dust again with the same method. After I precipitate the gold, stannous showed this color again. When this sponges showed up after sodium chlorate, stannous turned negative.


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## Yggdrasil (Mar 2, 2021)

I could not find the link just now, so I hope I'm forgiven.
This picture comes from one of LazerSteves threads.



And this for Rhodium from same thread



I can't see any of these colors in your test..
Do anyone else have an input here?


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## kurtak (Mar 2, 2021)

The method you are using to precipitate Pd from a solution "requires" the solution to be very concentrated

The reason for that is that you are trying to precipitate the Pd as a salt and that salt is actually water soluble

So if the solution has water in it - and depending on how much water is in the solution - you "may" get "some of the salt to precipitate - or it may not precipitate at all

You posted -------



> When I see dark brown color at stannous.



And then you also posted --------



> Then I saw brown with stannous. It is a like caramel color.



That is NOT the right the right color for a positive Pd stannous test

A positive Pd stannous test should show up as a dark green --- when you first do a Pd test with stannous it will show a orange/red color but will then quickly turn to a dark green (think forest green) there is such a thing as a "false" positive for Pd - but that will show up as a "light" green (think lime green)

So if your stannous test is brown it is likely not Pd

When you do a stannous test - and you THINK it is Pd --- you should ALWAYS follow the stannous test up with a DMG test --- other wise you can end up chasing your tail looking for Pd that just is not there

There are a number of false positive stannous test that you can get which I posted about here

:arrow: Cement

read that post as well as the one right after that one

Kurt


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## kurtak (Mar 2, 2021)

Yggdrasil said:


> I could not find the link just now, so I hope I'm forgiven.
> This picture comes from one of LazerSteves threads.
> 
> Au_Pt_Pd_Stannous.jpg
> ...



Thanks for posting that Yggdrasil - I have been looking for those pics recently to put in some of my other replies in other threads & was unable to find them 8) 

Kurt


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## Rotz (Mar 2, 2021)

Thank you guys, I have a question. 

Platinum & palladium salts can turn to type of in AR again? I mean If I change my mind after see platinum or palladium salt then can I turn back to solution then can I choose cementation method. Is this possible?


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## Lou (Mar 2, 2021)

Redissolution is an option on the ammonium-containing salts with great heating and concentrated aqua regia it is possible to oxidize the ammonium (NH4+) cation and even the ammonia ligand (NH3). It is not a recommended practice whatsoever because of the NOx formation, the misting, and the risk for NCl3 production in certain circumstances.


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## Rotz (Mar 3, 2021)

I see. Another question
Platinum salt doesn't dissolve in HCl as I read. When I dissolve in water. Should it make stannous positive ?

Palladium salt can dissolve HCl and water. Dissolved salt in these solutions should have make stannous positive?

Learning something neither too easy nor too hard if you have a lot of question in mind.


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## Yggdrasil (Mar 3, 2021)

Just happy to give back some Kurtak!


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## Rotz (Mar 5, 2021)

Hello

I tried drying the sponges. Then burn. Then melt. But just green residue I have. Then I learn purifying with ammonia. Remain material added ammonia. I saw very blue solution. Then add hcl. This is result.




I will purify with ammonia again. I bought dmg. Tomorrow check with dmg.

This title very nice to learn;
PGM Recover & Refining: Unknown green powder precipitated

Pd purifying in pictures


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## Rotz (Mar 6, 2021)

Hello 
To the conclusion, I dissolve the colorful sponge with ammonia again. Then I precipitate wlth dmg. I dont know why but it didnt precipitate as yellow sponge. I roast. Now I am searching pot to melt.


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## Yggdrasil (Mar 6, 2021)

I have not seen a positive stannous test yet, do you have any PMs in solution at all?


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## Lino1406 (Mar 7, 2021)

Green hue is either copper or nickel what is the pH?


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## Rotz (Mar 7, 2021)

Hello, ph level close to 5. I need support to ph adjustment when to take palladium from hcl, nitric, AR solution with DMG. Which alkaline should use for which solution. 

These dust treated in ammonia and Hcl. I applied DMG at second treatment with Ammonia. 

I cant melt yet. 


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## Lino1406 (Mar 7, 2021)

For DMG palladium, pH 4 - 4.5
For DMG nickel pH 8. Add ammoniak to the green mass, may turn to red (nickel)


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## kurtak (Mar 7, 2021)

In your very first post you said



Rotz said:


> I took black powder from my stock pot, saturated with copper. Then with AR I took the gold. When I see dark brown color at stannous.



Then you also posted



> Then I precipitate the gold with copperas. Then I saw brown with stannous. It is a like caramel color. Then I added ammonium chloride. Nothing happen and stannous show still same color. I add a lot of when the solution about 40 C. Nothing show up. Stannous still same.



Per the things I underlined in the above quotes --- I already said it once & I will say it again - THAT IS NOT a positive for Pd !!! --- in fact - a brown stannous test is NOT a positive for any precious metal --- a brown stannous result is a FALSE positive - brown can/will show up as a result of any number of metals &/or chemicals in a solution

The most common brown stannous is when to much SMB was used to drop the gold - if there is no copper in the solution it will be a lighter brown - if there is copper in solution it may show up as a darker brown due to the stannous reducing some copper

It (brown) can also be the result of iron in solution --- therefore - if you use copperas to drop your gold - & like SMB if you use more copperas then needed to drop your gold you can get a brown stannous test result

There are a number of "other" false positives you can get with stannous - I already provided you with a link about false positives - but here is that link again ---------

:arrow: Cement

Did you read that link ?

Yggdrasil posted a picture showing the color for Pd & I posted "in detail" about the color for a positive Pd stannous test --- The color for Pd is GREEN a deep dark green (like forest green) not a light green (like lime green (which is a false positive)

you posted ---------



> By the way I know false positive result. It is not that.



SMB is not the only false positive you can get with stannous - I have now posted - in detail - about the MANY false positives you can get with stannous

Do you now understand that your very first stannous test was more then likely a "false positive" & likely not a positive for Pd --- even if you did THINK there was Pd - at the very beginning - your very next test should have been a DMG test in order to confirm that you THOUGHT there was Pd in solution - or - sent it back to the stock pot to cement it with copper (again) - or - even cemented it with zinc which would have given you back copper & Pd (IF there was Pd) which could have then been re-dissolved which would have then given you a better/cleaner stannous test - to confirm what you thought "might" be Pd

At this point - in my opinion - you are doing nothing other then chasing your tail "hoping" to get something that is more then likely is NOT THERE - AND - in the process of chasing your tail AND you are doing nothing other then making a VERY TOXIC chemical soup !!!

So far you have a TOXIC chemical soup of HCl + nitric (= AR) + copperas + ammonium chloride + sodium chlorate + ammonia & now DMG & at this point you have got back NOTHING that even comes close to the Pd you are hoping &/or looking for

So my question to you is --- How much more time are you going to spend chasing something that more then likely just is not there - &/or how many more TOXIC chemicals are you going to continue to play with to make even more TOXIC waste --- as you chase something that more then likely is not there - & - what are you now going to do with all the TOXIC waste you have already created chasing something that more then likely is not there ??????

Bottom line here --- STOP chasing your tail & STOP making more TOXIC waste (that is slowly but surely poisoning you) with the HOPE that you will get something back - that likely is not there !!!

KURT


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## kurtak (Mar 7, 2021)

Lino1406 said:


> For DMG palladium, pH 4 - 4.5
> For DMG nickel pH 8. Add ammoniak to the green mass, may turn to red (nickel)



Lino - this is the first time I have heard about a Ph of 4 - 4.5 to precipitate Pd with DMG

I have precipitate quite a bit of Pd with DMG (both AR & nitric solutions) - I have always done it in a Ph 1 (acidic) solution which has always given me back the nice clean canary yellow DMG/Pd precipitate

Higher (then 1) Ph can/will cause other metals to precipitate - which - IF - there is Pd - can/will co-precipitate with the Pd - which would mean you need to take steps to clean up the multi metal (DMG) precipitate to get back to a clean Pd - if Pd precipitated with other metals

Or am I wrong about that ?

Kurt


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## Rotz (Mar 7, 2021)

Thank you for information. Sorry for no clear stannous test. It changed. When I share this post stannous color changed. So it is not what I see at the color. I also saw brown color. It was like middle brown like below. This stannous coming from same material before precipitate gold. I found records. 

Please comment me. I am chemist. I give my waste to the chemical waste recycler. 




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## Rotz (Mar 7, 2021)

kurtak said:


> Lino1406 said:
> 
> 
> > For DMG palladium, pH 4 - 4.5
> ...


My dmg doesnt work at ph 1. Firstly they show a little bit dust then they disappearing..


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## Lino1406 (Mar 7, 2021)

From my experience, if Pd is not pure or very diluted, best response to DMG is at pH 4-4.5. Literature gives 1-2 with high concentration, 1-6 otherwise


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## kurtak (Mar 8, 2021)

Rotz said:


> I give my waste to the chemical waste recycler.



That is good to know - thank you for dealing with you waste in a responsible way



> It was like middle brown like below.



you keep talking about the brown color with your stannous test

as I have posted - there are several reasons why you can get a brown result with a stannous test - but they are ALL false positives

Yggdrasil posted a picture of a true positive Pd - its GREEN - dark green

Here is another picture of a Pd stannous test - it's GREEN - dark green

:arrow: Pd purifying in pictures

If you have Pd in solution THAT green is going to be what you see when you do the stannous test --- if you do not see THAT green - you do NOT have Pd in solution

When you do the stannous test - if the Pd is very concentrated in the solution the "green" will show up instantly

If the solution is more diluted - when you first do the stannous test - it will "first" show up orange - the very same orange for Pt like the Pt test shown in the picture Yggdrasil posted - BUT - if it is Pd the orange will "very quickly" turn to the Pd green

Bottom line - if you do not see the green in these two pictures - YOU DO NOT HAVE Pd in your solution

Kurt


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## g_axelsson (Mar 8, 2021)

Another positive Pd test.

I dip the cotton top in my solution and put a drop of stannous on the top so I can see the reaction between the solution and stannous as a zone. And the colors change over time. But that green is a positive reaction.




Göran


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## Rotz (Mar 8, 2021)

Hello 
I will dissolve and check again precipitated dust. What about this colors. I took from kadriver’s video





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## kurtak (Mar 9, 2021)

Rotz said:


> Hello
> I will dissolve and check again precipitated dust. What about this colors. I took from kadriver’s video
> 
> eda6b61a-dfa9-4a1d-a86a-7a94ba9c88c1.jpg
> ...



I have no idea what is going on with that picture - but something is not right - I say that because even the gold test does not look gold positive --- the gold test should be a very clear PURPLE color (in low concentration of gold) or even BLACK (with high concentration of gold) but instead the gold test in that picture looks a reddish brown --- even the Pt test looks off in its color (its orange but it should be a very "bright" orange not a dull orange) --- therefore I simply do not trust that picture as good &/or true examples of stannous tests for those metals

What I do know - over the years of refining I did - I worked with a "fair" amount of Pd - Pd in both AR & nitric solutions - solutions of "high" Pd concentration & "low" Pd concentration - solutions that were very Pd clean & solutions that were very dirty (more other/base metals then Pd) --- EVERY stannous test I every did produced the very evident Pd GREEN test result - NEVER some other color

That is the whole purpose of doing a stannous test - the metals we test for have a VERY clear & evident color to them that can not be mistaken - those colors are --- Au = PURPLE --- Pt = ORANGE --- Pd = GREEN

If you do not get those colors you more then likely DO NOT have those metals in solution

you can get OTHER colors with stannous - BUT - even with other colors - if Au - Pt or Pd is in solution - the colors for those metals will show up in the test - separate from the other colors

The picture Goran posted is a good example of that --- in that picture there are three different colors - they are all separate from each other & the reason he knew there was Pd in the solution was the GREEN was separate from the other two colors

Bottom line - when you do a stannous test - if you don't get Au PURPLE - Pt ORANGE or Pd GREEN then those metals more then likely just are not in solution --- no mater how much you want them to be in solution

The ONLY one that can fool you is the Pt test - & that is because molybdenum will give you an orange test result that is VERY close to the orange of Pt

Kurt


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## kurtak (Mar 10, 2021)

Rotz said:


> My dmg doesnt work at ph 1. Firstly they show a little bit dust then they disappearing..



How are you adding your DMG ?

Are you just putting it in as a powder - or are you dissolving it first ?

If dissolving it first how are you dissolving it ?

per the underlined - Pd precipitated with DMG does NOT re-dissolve in acid --- so - if you add DMG to a Ph1 solution - and there is Pd in (the acidic) solution - then the Pd is going to precipitate as the canary yellow DMG/Pd & remain precipitated

That is the very reason why we use DMG to confirm that Pd is in (an acidic) solution - DMG is selective to PD ONLY in Ph 1 acidic solutions - therefore if you do not get the canary yellow precipitate when adding DMG to an acidic solution --- YOU DO NOT HAVE Pd in solution 

If you have other metals in solution (acidic) then you MAY get something to precipitate when you first add the DMG - but - that precipitate will then re-dissolve --- that is especially true if you use NaOH to dissolve the DMG --- The NaOH will precipitate the other metals when you first add the DMG - but the acid will then re-dissolve those NaOH precipitates --- then IF Pd is in solution - only the canary yellow Pd will precipitate & STAY precipitated

Therefore - when you start raising the Ph - the more you raise it - the more likely you are to start precipitating OTHER metals & having them stay precipitated 

In other words - If Pd did not precipitate at Ph 1 - then there is NO Pd --- raising the Ph in NOT going to change that - it is only going to cause OTHER metals to precipitate

Bottom line - you "never" got a Pd positive "green" result with your stannous test - but you still thought you "might" have Pd in solution --- so now you tried using DMG in a Ph 1 solution - you did not get the canary yellow Pd to precipitate - therefore the two test that are used to confirm if Pd is in solution have failed :!: 

Therefore - you now know for absolutely sure that you DO NOT have Pd in solution :!: 

So STOP chasing something that is very clearly NOT THERE :!: 

Because you have now used the two test that are used to determine if Pd is in solution (or not) & both of those test have failed :!: 

Kurt


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## Rotz (Mar 10, 2021)

Hello

Thank you Kurt. Why your response looks sharp and nervous. I m very respectful everybody’s help trying. I doubt whether may I misunderstood because of my insufficient english. 
Anyway, I am here to learning. This is palladium positive test 
A








What is this platinum or fake?
B






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## acpeacemaker (Mar 10, 2021)

I've read through this entire drawn out post. But can you just say what your main feedstock was that you have processed? That your stockpot acquired "said powders" from?


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## kurtak (Mar 11, 2021)

Rotz said:


> This is palladium positive test



Is that a stannous test ?

or is it a DMG test ?

What is the solution Ph of that test ?



> What is this platinum or fake?



Same questions as above

Kurt


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## Rotz (Mar 12, 2021)

acpeacemaker said:


> I've read through this entire drawn out post. But can you just say what your main feedstock was that you have processed? That your stockpot acquired "said powders" from?



Yes, I proccessed black powders form bottom of the vessel.


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## Rotz (Mar 12, 2021)

kurtak said:


> Rotz said:
> 
> 
> > This is palladium positive test
> ...




They are stannous test. I didn't apply DMG. I saw deep forest green when add the stannous to photo A like around of the solution at the spoon. Then it turn to orange like middle of the solution.

Photo B another solution It is very bright yellow. It can be wrong result. All I need to know learn what I see with your comment. 

Thank you.


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## acpeacemaker (Mar 12, 2021)

Rotz said:


> acpeacemaker said:
> 
> 
> > I've read through this entire drawn out post. But can you just say what your main feedstock was that you have processed? That your stockpot acquired "said powders" from?
> ...



Hi Rotz,

Sorry this might be the language barrier thing. But I'm asking what have you been refining altogether to get those powders. Escrap, karat, ore, braze, sand, auto, etc. Is there a main subject material in particular you have recovered from that eventually goes into and accumulates your stockpot.


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## kurtak (Mar 12, 2021)

Rotz said:


> They are stannous test. I didn't apply DMG. I saw deep forest green when add the stannous to photo A like around of the solution at the spoon. Then it turn to orange like middle of the solution.
> 
> Photo B another solution It is very bright yellow. It can be wrong result. All I need to know learn what I see with your comment.
> 
> Thank you.



Very good & thank you for answering my questions --- it looks like we MAY have found your Pd  

Now - don't doing anything with the solution you took those test from yet

That is because we FIRST want to do a little more testing to "confirm" the Pd is really there :!: 

Then - once we confirm that (with some more testing) we will work at getting that Pd back for you so that you will have a product that has real value

I don't have time to post more today - so will post more tomorrow --- this will likely take a few days of talking back & forth so that getting your Pd is done right this time ---(if in fact the Pd is there)

Kurt


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## kurtak (Mar 12, 2021)

acpeacemaker said:


> Rotz said:
> 
> 
> > acpeacemaker said:
> ...



Yes - although we do not need that info to solve this - it would certainly be helpful to have that info --- so good question 

Kurt


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## Rotz (Mar 12, 2021)

acpeacemaker said:


> Rotz said:
> 
> 
> > acpeacemaker said:
> ...


Sorry it is my bad. All of them from e scrap. Mainly ram and cell phone. Today I read a little bit Hoke. I undertood my faults. I applied ammonium chloride to hot solution. And sodium chlorate. So base metal contamination been very much. 

Also Dmg precipitate something because of the NaOH. I used min amount NaOH but I guess it increase of PH. Then I saw precipitating. Actually I calculate before precipitation to pd amount according to DMG amount. It came like my calculated amount,luck in to issue. (unluckyness)

By the means of this post I learnt the stannous positive result. In order to trusting kadriver post, I process my solution with him photo. I dont know maybe still his photo true but for different condition. I am gonna be more careful. Something dont learn without trying. I know it is dangerous but I have lab experiment from school. I know acid treatment or precipitaion or using equipment. 

Thank you for helping. 


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## Rotz (Mar 12, 2021)

I also proccessed hdd board and blue capacitor about 1 kg. 


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## Yggdrasil (Mar 12, 2021)

Rotz.
I'm sorry to say so, but in most modern e-waste there are no to little Pd.
The exeption is high end serverboards and some other high end boards.
So unless you had a "ton" of these HDD boards I don't expect there are much Pd at all.
Which acidentally are what the tests show.

So if you already have your gold out, i would let the waste liquor go to the stock pot and redissolve the rest of the powders/waste that is left (to ensure nothing is left in there) and put that to the stock pot too.
If there is any kind of value in there you will get it when you process your stock pot.


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## kurtak (Mar 13, 2021)

Rotz said:


> They are stannous test. I didn't apply DMG. I saw deep forest green when add the stannous to photo A like around of the solution at the spoon. Then it turn to orange like middle of the solution.
> 
> Photo B another solution It is very bright yellow. It can be wrong result. All I need to know learn what I see with your comment.
> 
> Thank you.



Then I answered 



> Very good & thank you for answering my questions --- it looks like we MAY have found your Pd
> 
> Now - don't doing anything with the solution you took those test from yet
> 
> That is because we FIRST want to do a little more testing to "confirm" the Pd is really there



Ok - so - hopefully you have not actually done anything with the solution you took those test from yet ?

Please answer that question

Then - as long as you have not done anything with that solution I need to know --------

Is it a nitric acid only solution --- or a HCl only solution --- or an AR solution 

Then - I want to see a picture of that solution ( a picture of the actual solution in the beaker)

Then I want you to do 2 more stannous test - I want you to do those test in a different way then the way you have been doing them

Instead of doing the test in a spoon like you have been doing I want you to do this ---------

Test 1) use a cotton swab (like in the picture that Yggdrasil & Goran posted) - dip it in the solution so the cotton gets wet - then put "one" drop of stannous on the cotton swab that was dipped in the solution --- then take a picture of that test & show it to us

Test 2) on a paper filter (or a paper towel if you don't have paper filters) put two different drops of the solution - one drop - then another drop next to the first - with some room between the two drops --- then on one of those drops put a drop of stannous - but do not put any stannous on the other drop --- take a picture of that test & show it to us 

Once you answer my questions & post the pictures I asked for we will move on to the next step(s) of what to do

Kurt


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