Input on Precipitation with ammonium chloride

[eshane211]

Hello hope all is well!! I precipitated this beautiful material from a suspected highly saturated palladium solution with a saturated ammonium chloride solution. it actually appears more orange in person. The material I started with is what I believe is high grade complex ore which i stumbled upon about 2 1/2 years ago. i have been researching, learning and trying to figure out what it is exactly that i have found. i haven't been able to cover the costs of any testing or assaying and have not found anyone willing to help even after going to 4 separate colleges. its been challenging but its been so much fun and i appreciate the knowledge and input!!

 

[Platz]

Looks like ammonium chloroplatinate, what colour was your solution before and after dropping?

 

[Lino1406]

Ammonium hexachloro platinate has very low solubility in water. Check it. Also check solution with stannous chloride

 

[kurtak]

from a suspected highly saturated palladium solution

Per the bold print - what do you mean "suspected" --- didn't you first test the solution with stannous ? - & then confirm with DMG ?

Kurt

 

[butcher]

I find this suspicious, without details, please tell us more.

 

[orvi]

Hello hope all is well!! I precipitated this beautiful material from a suspected highly saturated palladium solution with a saturated ammonium chloride solution. it actually appears more orange in person. The material I started with is what I believe is high grade complex ore which i stumbled upon about 2 1/2 years ago. i have been researching, learning and trying to figure out what it is exactly that i have found. i haven'tView attachment 54323View attachment 54324View attachment 54325View attachment 54326View attachment 54327 been able to cover the costs of any testing or assaying and have not found anyone willing to help even after going to 4 separate colleges. its been challenging but its been so much fun and i appreciate the knowledge and input!!

If you have platinate there - it would be easy to test. Test it with stannous chloride and you will see bright orange colour - that is positive for Pt and it is quite sensitive.

Precipitating palladium with ammonium chloride is unlikely in standard conditions - you will need to harshly oxidize the solution further by adding sparging with chlorine, or adding sodium chlorate. Ammonium hexachloropalladate is brick red coloured, so this won´t be it.

Also, I do not like the shape and colour of the crystals - (NH4)2PtCl6 has very low solubility in acidic media containing excess NH4Cl and precipitates as fine precipitate. In order to obtain crystals, you would need to crystallize it from boiling water - and concerning low solubility (ca 30g/L), you got crystals approximately sized as finer crystal sugar - with them being very deep orange colour.
I would say there could be some ammount of Pt in the solution, but the rest of the bulk being ammonium chloride crystallizing out together with traces of Pt - if there is Pt.

Do that simple test (SnCl2 is a must, and it is practically free to do). If the yellow colouration is indeed Pt, you will obtain very strong positive from stannous. Remember to test acidic solution, it won´t work neutral or basic.

 

[eshane211]

If you have platinate there - it would be easy to test. Test it with stannous chloride and you will see bright orange colour - that is positive for Pt and it is quite sensitive.

Precipitating palladium with ammonium chloride is unlikely in standard conditions - you will need to harshly oxidize the solution further by adding sparging with chlorine, or adding sodium chlorate. Ammonium hexachloropalladate is brick red coloured, so this won´t be it.

Also, I do not like the shape and colour of the crystals - (NH4)2PtCl6 has very low solubility in acidic media containing excess NH4Cl and precipitates as fine precipitate. In order to obtain crystals, you would need to crystallize it from boiling water - and concerning low solubility (ca 30g/L), you got crystals approximately sized as finer crystal sugar - with them being very deep orange colour.
I would say there could be some ammount of Pt in the solution, but the rest of the bulk being ammonium chloride crystallizing out together with traces of Pt - if there is Pt.

Do that simple test (SnCl2 is a must, and it is practically free to do). If the yellow colouration is indeed Pt, you will obtain very strong positive from stannous. Remember to test acidic solution, it won´t work neutral or basic.

I don't believe I initially had my stannous chloride recipe correct. But there was some slight yellow appearing. you are right on with the larger crystals in that batch since the first time I precipitated this material I was attempting to dry it out a bit but it liquified so I then cemented it out on tin. I then wanted to see what the solubility of the cemented material was and it to dissolved very easily but upon cooling precipitated again and again larger crystals formed.

These are the much smaller and have only been precipitated with ammonium chloride. I did rinse the one on the right with dilute hydrochloric and managed to not have it dissolve. I'm not sure if that's what gave it the slightly deeper orange or if that was a difference because of the ore These are 2 separate batches of suspected ore. The batch with larger crystals is a 3rd batch.

 

[eshane211]

Looks like ammonium chloroplatinate, what colour was your solution before and after dropping?

Solution goes from brownish to yellow orange and finished with light yellow greenish.

 

[eaglekeeper]

It's hard to mess up making stannous chloride..... some say it can go bad. I've been using the same stannous batch for nearly 2 years and still works fine, so I don't know what the shelve life is. Chances are your original stannous test was probably correct.

Putting ore with unknow content into acid can be bad for your/others health. Most metals that are completely safe in there elemental form can be quit toxic when dissolved. Once dissolved, they are more readily absorbed into the skin and air way linings (fumes)... wear protective gear.

 

[orvi]

I don't believe I initially had my stannous chloride recipe correct. But there was some slight yellow appearing. you are right on with the larger crystals in that batch since the first time I precipitated this material I was attempting to dry it out a bit but it liquified so I then cemented it out on tin. I then wanted to see what the solubility of the cemented material was and it to dissolved very easily but upon cooling precipitated again and again larger crystals formed.
View attachment 54331
These are the much smaller and have only been precipitated with ammonium chloride. I did rinse the one on the right with dilute hydrochloric and managed to not have it dissolve. I'm not sure if that's what gave it the slightly deeper orange or if that was a difference because of the ore These are 2 separate batches of suspected ore. The batch with larger crystals is a 3rd batch.

As ammonium hexachloroplatinate isn´t very soluble in HCL, note that also ammonium or sodium chloride aren´t very soluble in HCL too.
Colour in the bowl on the left is right, and there aren´t many inorganics which will form this kind of precipitate from aqueous solutions with chemicals used.
So chances are you actually can have platinate salt.
Take a sample and digest it in AR. This help to form a solution, as salt itself has very poor solubility in water. Take a drop of this digested sample and add SnCl2 to it. Recipees for SnCl2 are here on the forum. Stannous will work in very wide concentration range - and that colouration for Pt is very distinct. Colour will change from yellowish (dissolved sample) to nice orange.


These photos show the sample of dilute and more concentrated PtPd solution. Green colouration is from Pd, orange from Pt. Original sample was nearly transparent (left), very pale yellow. On the right, original sample was yellowish in colour. That colour change is unmistakeable
Ignore that green colouration, and this is what you should see upon addition of SnCl2 test.

 

[eshane211]

can anyone please tell me what a good next step would be to take to turn the salts to a form someone would purchase. I do also have some incredible ore pieces once I can prove it is in fact what I know it to be. Any next step with that would also be greatly appreciated!! Thanks again and as always I am doing everything in my power to be as safe and informed as I possibly can to protect my self and others!!

 

[Lino1406]

I don't believe I initially had my stannous chloride recipe correct. But there was some slight yellow appearing. you are right on with the larger crystals in that batch since the first time I precipitated this material I was attempting to dry it out a bit but it liquified so I then cemented it out on tin. I then wanted to see what the solubility of the cemented material was and it to dissolved very easily but upon cooling precipitated again and again larger crystals formed.
View attachment 54331
These are the much smaller and have only been precipitated with ammonium chloride. I did rinse the one on the right with dilute hydrochloric and managed to not have it dissolve. I'm not sure if that's what gave it the slightly deeper orange or if that was a difference because of the ore These are 2 separate batches of suspected ore. The batch with larger crystals is a 3rd batch.

Cementing with tin is not usual, so there is very low platinum, if any. This is also supported by the fact that the yellow precipitate was readily dissolved in water.

 

[eshane211]

Cementing with tin is not usual, so there is very low platinum, if any. This is also supported by the fact that the yellow precipitate was readily dissolved in water.

I believe it is palladium which will dissolve in water and not platinum. There was no aqua regia used so platinum would not be in my solution

 

[Yggdrasil]

I believe it is palladium which will dissolve in water and not platinum. There was no aqua regia used so platinum would not be in my solution

No Precious metal will dissolve in water!!
Palladium will dissolve in Nitric, Aqua Regia, HCl/Cl, HCl/Peroxide or similar, but NOT water.
The salts of most precious metals will dissolve in water though.

 

[eshane211]

No Precious metal will dissolve in water!!
Palladium will dissolve in Nitric, Aqua Regia, HCl/Cl, HCl/Peroxide or similar, but NOT water.
The salts of most precious metals will dissolve in water though.

I meant that the salts dissolved in water not the ore

 

[Yggdrasil]

I meant that the salts dissolved in water not the ore

Almost all, if not all Chlorides of PMs dissolve easy in water.
The Ammonium salts on the other hand don't always dissolve easy.
Testing with Stannous i imperative before treating a solution.
There is no need for a recipe of Stannous, dissolve some Tin in HCl and you have Stannous.

Have you read C.M. Hokes book?
Or the safety section of the forum?
Or dealing with waste?

 

[Lou]

Why doesn't the original poster back up about 100 steps and tell us what he did after he tells how much he started with and why he thinks it's got PGM in it? Maybe even putting a rough geological location, the history of the "ore", etc. would be helpful.

Right now this is, "help me, I have a yellow powder that could/can be anything but I think it's palladium for no real reason other than I believe it to be complex ore I stumbled on 2 and 1/2 years ago." "I believe it is palladium which will dissolve in water and not platinum. There was no aqua regia used so platinum would not be in my solution"

I believe it to be yellow stuff with crystals in it. That's what this deserved.

I think it's time for a crack down on these types of posts. Still, for all anyone knows, it's cis-diamminopalladium (II) chloride he made which is the result of boiling Pd chlorosolutions with ammonium chloride and urea for hours and hours.

So, eshane211:

How much ore did you put into _________ and what quantity of __________ did you use? What was the concentration of ______ that you used?
Did you heat it or did it get hot? How long? What color changes happened? Did any bubbling occur or gases seem to be released?
When you added the ammonium chloride to the mother liquor solution which was dark brown in color, how long did it take before the colors changed?
If you put a piece of copper wire in a sample of the the solution, does a grey or black colored deposit form immediately?
When you add excess ammonia water to a small sample of the precipitate, does it dissolve? What colors does it make?

 

[eshane211]

Why doesn't the original poster back up about 100 steps and tell us what he did after he tells how much he started with and why he thinks it's got PGM in it? Maybe even putting a rough geological location, the history of the "ore", etc. would be helpful.

Right now this is, "help me, I have a yellow powder that could/can be anything but I think it's palladium for no real reason other than I believe it to be complex ore I stumbled on 2 and 1/2 years ago." "I believe it is palladium which will dissolve in water and not platinum. There was no aqua regia used so platinum would not be in my solution"

I believe it to be yellow stuff with crystals in it. That's what this deserved.

I think it's time for a crack down on these types of posts. Still, for all anyone knows, it's cis-diamminopalladium (II) chloride he made which is the result of boiling Pd chlorosolutions with ammonium chloride and urea for hours and hours.

So, eshane211:

How much ore did you put into _________ and what quantity of __________ did you use? What was the concentration of ______ that you used?
Did you heat it or did it get hot? How long? What color changes happened? Did any bubbling occur or gases seem to be released?
When you added the ammonium chloride to the mother liquor solution which was dark brown in color, how long did it take before the colors changed?
If you put a piece of copper wire in a sample of the the solution, does a grey or black colored deposit form immediately?
When you add excess ammonia water to a small sample of the precipitate, does it dissolve? What colors does it make?

ok so i started a fresh test batch and have photographed my way through it so far with each step no heating has been needed:

I have started with a 58.2 gram sample of suspected complex ore. i decided to try processing the palladium first because i suspected it was what the sample contained the most of and I had previously attempted other steps unsuccessfully



Filled my plastic container halfway up with my concentrated acid solution. reacted immediately I screwed top on but watched for gas buildup and released a few times during process



I shook the material often being very careful to make sure my container had a good tight seal so it didn't come pouring out onto my hands even though gloves should be a must for these projects. I took these an hour in:



Tested with my stannous chloride. The result was a light yellow with a slight green tint but so is my solution and my stannous so unsure with color but also particles fell out to the bottom



Photos after approximately hour 2 will have to be in the next post im actually coming up to hour 3 so im gonna go check I added a bit of fresh acid and let that do its thing im gonna filter and then test 2 seperate methods. Hope everyone has a wonderful everything and ill be back with an update once completed!!

 

[Yggdrasil]

ok so i started a fresh test batch and have photographed my way through it so far with each step no heating has been needed:

I have started with a 58.2 gram sample of suspected complex ore. i decided to try processing the palladium first because i suspected it was what the sample contained the most of and I had previously attempted other steps unsuccessfully

View attachment 54344View attachment 54345View attachment 54346View attachment 54347

Filled my plastic container halfway up with my concentrated acid solution. reacted immediately I screwed top on but watched for gas buildup and released a few times during process

View attachment 54350View attachment 54351View attachment 54352View attachment 54354

I shook the material often being very careful to make sure my container had a good tight seal so it didn't come pouring out onto my hands even though gloves should be a must for these projects. I took these an hour in:

View attachment 54354View attachment 54355View attachment 54356View attachment 54357View attachment 54358View attachment 54361View attachment 54360

Tested with my stannous chloride. The result was a light yellow with a slight green tint but so is my solution and my stannous so unsure with color but also particles fell out to the bottom

View attachment 54362View attachment 54363View attachment 54364View attachment 54365View attachment 54366View attachment 54367View attachment 54368

Photos after approximately hour 2 will have to be in the next post im actually coming up to hour 3 so im gonna go check I added a bit of fresh acid and let that do its thing im gonna filter and then test 2 seperate methods. Hope everyone has a wonderful everything and ill be back with an update once completed!!

What kind of assay do you have of the ore?
And tell me you have read the book and the appropriate sections in this forum?

 

[eshane211]

What kind of assay do you have of the ore?
And tell me you have read the book and the appropriate sections in this forum?

I haven’t been able to afford the cost of an assay hence the backyard lab that isn’t my first choice but for the last 2 years seems to be my only choice. I can’t even begin to explain the amount of research I have done and I have read hokes book and printed it and have been rereading followed by some more researching