bunch of questions about silver chloride

[mikeman001]

No black upon lye addition, correct? Same issues here...I think that might be brass or nickel, probably brass... I suspect that the nickel layer is as thick as the silver that tops it.... Once the brass is exposed(on some) I'm leaning towards a heavy contamination of nickel and then brass.... Out of 200g. Of reverse electroplated "silver powder" , so far I've got roughly 32g. Of silver melted down and somewhat"clean"... So far... With a heavy brass/copper presence to clean along the way...

Almost positive I left the hydro cell running too long per piece of sliver played platters

 

[mikeman001]

 

[mikeman001]

 

[J.Najam]

I like that silver you posted above,

But i think my post may misleading.

Can anyone tell me what this ?

This is the sludge I have post decantation process. Could this be silver or am I wasting my time tryimg to further decant and recover if any PM?

This is basically the decanted solution and solvent of the decanted water container. Silver granules are in a different beaker, kept aside. This is what i got from the decanted water bucket. Now im not sure if this contains any silver or may be im just wasting my time after the wrong thing..

 

[Yggdrasil]

Can anyone tell me what this ?

This is the sludge I have post decantation process. Could this be silver or am I wasting my time tryimg to further decant and recover if any PM?

I do not know for sure, but I guess it is a mix of unreacted Silver Chloride, Silver Oxide and different organics and Hydroxides.
I really do not know if it is worth collecting.
If you are going to process more Silver in the future you can collect it and smelt it when you have acquired a decent batch. Maybe you can find a few grams, but I doubt it will be worth it alone.

 

[mikeman001]

I like that silver you posted above,

But i think my post may misleading.

This is basically the decanted solution and solvent of the decanted water container. Silver granules are in a different beaker, kept aside. This is what i got from the decanted water bucket. Now im not sure if this contains any silver or may be im just wasting my time after the wrong thing..

I've had the same material decanted as well. I tried to oxidize and the color was greenish brown, no black. Just to see if any would come of it, even added sugar for the underworld of it... that part of it was not fruitfull

 

[J.Najam]

I do not know for sure, but I guess it is a mix of unreacted Silver Chloride, Silver Oxide and different organics and Hydroxides.
I really do not know if it is worth collecting.
If you are going to process more Silver in the future you can collect it and smelt it when you have acquired a decent batch. Maybe you can find a few grams, but I doubt it will be worth it alone.

Hmm, Ill do exactly as you said. Save it. And see if it can be done in future. This sediment now rests in a beaker with some water out in the scorching sun to dry it out. God knows how long that takes. Ill store the powders and see it later on

 

[J.Najam]

I've had the same material decanted as well. I tried to oxidize and the color was greenish brown, no black. Just to see if any would come of it, even added sugar for the underworld of it... that part of it was not fruitfull

Did you try treating it exactly the way we process after achieving silver chloride?

 

[mikeman001]

Did you try treating it exactly the way we process after achieving silver chloride?

Yes sir, sodium hydroxide followed by sugar addition... Behaved differently, however. Color wasn't rite and nothing precipitated.

 

[J.Najam]

Behaved differently

I would suggest if you could elaborate this observation, it woule be easier for any experienced senior member to further break it down and make sense of however it can be treated.

For the time being I believe the best is what @Yggdrasil has advised. Maybe keep it aside and use for further silver refining operations. But before that hopefully someone can chime in who may have faced a similar difficulty at some point during their refining.

 

[J.Najam]

Hello again,

I was expecting around 25 somethimg grams of silver from the silver nitrate crystals after all the calculations. Turns out it was only 3.3? Could it be possible I did anything wrong anywhere?

 

[Yggdrasil]

Hello again,

I was expecting around 25 somethimg grams of silver from the silver nitrate crystals after all the calculations. Turns out it was only 3.3? Could it be possible I did anything wrong anywhere?

What was the weight of the Silver Chloride and the Silver Nitrate?
It is quite possible that you did not have a complete conversion.

 

[J.Najam]

What was the weight of the Silver Chloride and the Silver Nitrate?
It is quite possible that you did not have a complete conversion.

I did not weigh the chloride, but nitrate were 46 grams

 

[Yggdrasil]

I did not weigh the chloride, but nitrate were 46 grams

With perfect conversion you should have around 29 grams.
There are 3 places you can have these losses. Incomplete conversion to Silver Chloride including contaminated Silver Nitrate.
Incomplete conversion to Silver Oxide and then incomplete conversion to Silver.
Take a gram of the Nitrate, dissolve it and then add a few drops of Nitric before cementing it on Copper.
See how much you can reclaim after washing it well. Maybe in dilute Ammonium Hydroxide until it is colorless.
This will indicate the purity of the Nitrate.
If this do not have a significant loss then it is in the last two steps. Maybe convert with Sulphuric/Iron instead?

 

[J.Najam]

Incomplete conversion to Silver Oxide

I believe this is where I may have started messing it up.

drops of Nitric before cementing it on Copper

I dont have nitric at the moment. Would it be an issue if I just hang the copper in there after nitrate crystal dissolution? I am literally just thinking to put it aside and let the copper do its work. Shake the bar every now and then. Then wash and move forward.

Maybe convert with Sulphuric/Iron instead?

I would love to see a visual in this case. Because I think @kurtak mentioned somewhere earlier about the formation of iron hydroxides and its contamination which brought in my skepticism about proceeding with this.

around 29 grams.

Yep. 27.07 is what I got and seeing 3.3 just shook me up!

Edited for wrong calculation*

 

[lazersteve]

The other possibility is you overheated the melt and ran it way too long vaporizing the Ag in the melting stage.

It's even possible you didn't fully convert a large portion of the AgCl and it ended up in the flux/slag. Have you remelted your slag with excess soda ash at 550-900C? You may find the missing Ag doing this especially considering the AgCl and Ag2O are both solids and nothing should have become dissolved in the conversion process assuming you started with pure AgNO3 and did a complete conversion to AgCl in the beginning.

Steve

 

[Yggdrasil]

The other possibility is you overheated the melt and ran it way too long vaporizing the Ag in the melting stage.

It's even possible you didn't fully convert a large portion of the AgCl and it ended up in the flux/slag. Have you remelted your slag with excess soda ash at 550-900C? You may find the missing Ag doing this especially considering the AgCl and Ag2O are both solids and nothing should have become dissolved in the conversion process assuming you started with pure AgNO3 and did a complete conversion to AgCl in the beginning.

Steve

I do not think he has melted anything yet, at least not as per the description.
How is your take on the Sulphuric/Iron method?
He has a loss of about 90%, which seems to be impossible under normal situations.

 

[J.Najam]

other possibility is you overheated the melt and ran it way too long vaporizing the Ag in the melting stage.

Hello,

Thanks for your response,

I got the actual weight before the melting stage. It was the same after the melt as well. Could it be possible that it does vaporize during the drying stage? I left it on heat in a stainless steel bowl for drying on a hotplate. I can't figure out any other remaining possibility. Even then, I don't think I'd have vaporized 20 grams or so in the process?

It's even possible you didn't fully convert a large portion of the AgCl and it ended up in the flux/slag

I can very much agree with you guys on the conversion part, but I did not have any remaining slag. Again, It was melted in a smaller stainless steel bowl. There were no remains and it melted pretty fast on that though.

assuming you started with pure AgNO3

I assumed the same, but I'll repurchase it and retry with a different method. I was thinking a copper bar..

How is your take on the Sulphuric/Iron method?

But as emphasized on this, as much as I've read it. Any visual would be an icing on the cake

I do not think he has melted anything yet

Ah, I did not mention, but I did melt and it came out better than my gold. I tried re-melting my gold the same way as silver, but it did not result the same way and kind of became darker in the process

 

[Yggdrasil]

Hello,

Thanks for your response,

I got the actual weight before the melting stage. It was the same after the melt as well. Could it be possible that it does vaporize during the drying stage? I left it on heat in a stainless steel bowl for drying on a hotplate. I can't figure out any other remaining possibility. Even then, I don't think I'd have vaporized 20 grams or so in the process?

I can very much agree with you guys on the conversion part, but I did not have any remaining slag. Again, It was melted in a smaller stainless steel bowl. There were no remains and it melted pretty fast on that though.

I assumed the same, but I'll repurchase it and retry with a different method. I was thinking a copper bar..

But as emphasized on this, as much as I've read it. Any visual would be an icing on the cake

Ah, I did not mention, but I did melt and it came out better than my gold. I tried re-melting my gold the same way as silver, but it did not result the same way and kind of became darker in the process

Did you melt the Silver Chloride???
Because that was what I was refering to, because that can be done but it always lead to losses.

 

[J.Najam]

Did you melt the Silver Chloride???

No, just the powders directly.