Result of silver preciptation

[Robson]

Hellow My frends, i made a process with silver from contacts, in nitric acid, i preciptated with HCL, and a got a very strange result. i`ll be posting here the photos of something that looks more like a kind of crumbly biscuit, which after being melted does not react to acids agan. i really don`t know what it is, remembering that the silver also came ok.

 

[4metals]

Is there a question in your post? You did not say how you processed the Silver Chloride. You said how you converted the Silver nitrate to Silver Chloride but nothing about reducing the Silver Chloride. If it did not melt into a metallic bar you likely never reduced the Silver Chloride to metal and actually melted the chloride into crumbly biscuits to use your description.

A few more details and we can likely help you fix this.

 

[4metals]

Quite a few years back I ran a process which generated a lot of Silver Chloride and had in excess of 1% Gold in the mix. I melted the filtered and damp chlorides in a cool furnace not intending to exceed the 850° F the Silver Chloride melts at by too much. This avoided the copious smoke when refiners try to melt all the way to metallic Silver. This is a photo of one of the bars I still had lying around. (It’s amazing what old refiners find lying around!) Exposure to light has darkened it over the years but this is what a Silver Chloride “biscuit” can or should look like. The OP should note this bar would not be attacked with nitric acid.

The holes were drilled to sample it. The bars of Silver Chloride were brought down to about 1/4” chunks in a jaw crusher and placed in a ceramic ball mill with cast iron balls in a 10% solution of sulfuric acid.

What resulted was silver metal and smaller iron balls. The Silver metal was melted into anodes and the gold was recovered from the slimes.

 

[Robson]

Quite a few years back I ran a process which generated a lot of Silver Chloride and had in excess of 1% Gold in the mix. I melted the filtered and damp chlorides in a cool furnace not intending to exceed the 850° F the Silver Chloride melts at by too much. This avoided the copious smoke when refiners try to melt all the way to metallic Silver. This is a photo of one of the bars I still had lying around. (It’s amazing what old refiners find lying around!) Exposure to light has darkened it over the years but this is what a Silver Chloride “biscuit” can or should look like. The OP should note this bar would not be attacked with nitric acid.
View attachment 58158
The holes were drilled to sample it. The bars of Silver Chloride were brought down to about 1/4” chunks in a jaw crusher and placed in a ceramic ball mill with cast iron balls in a 10% solution of sulfuric acid.

What resulted was silver metal and smaller iron balls. The Silver metal was melted into anodes and the gold was recovered from the slimes.

then I realized that these "biscuits" darken in sunlight, the process resulted in a lot of "silver chloride" but when melting only part of it it melted into solid silver, the rest of it or I can say most of it turned into that, it is not attacked with nitric , and not even with agua regia. and it is similar to your result, so is it possible to recover it?
Thank you for your feedback, and I look forward to your response.

 

[Robson]

Is there a question in your post? You did not say how you processed the Silver Chloride. You said how you converted the Silver nitrate to Silver Chloride but nothing about reducing the Silver Chloride. If it did not melt into a metallic bar you likely never reduced the Silver Chloride to metal and actually melted the chloride into crumbly biscuits to use your description.

A few more details and we can likely help you fix this.

Good evening friend and sorry for the delay, thanks for your reply, answering how I obtained the silver, I dissolved the tips in nitric, and precipitated with HCL, metallized with SODIUM HYDROXIDE, and added a kind of molasses, which is nothing more than burnt sugar .

 

[Robson]

Good evening friend and sorry for the delay, thanks for your reply, answering how I obtained the silver, I dissolved the tips in nitric, and precipitated with HCL, metallized with SODIUM HYDROXIDE, and added a kind of molasses, which is nothing more than burnt sugar .

 

[Robson]

Is there a question in your post? You did not say how you processed the Silver Chloride. You said how you converted the Silver nitrate to Silver Chloride but nothing about reducing the Silver Chloride. If it did not melt into a metallic bar you likely never reduced the Silver Chloride to metal and actually melted the chloride into crumbly biscuits to use your description.

A few more details and we can likely help you fix this.

The resulting "COOKIE" does not react to nitric, nor to aqua regia, it reacts exposed to the sun, it darkens in a color similar to purple, which reminds me of the reaction of silver chloride when exposed to the sun, I would like to post a video of it here, but it does not load.

 

[Robson]

Is there a question in your post? You did not say how you processed the Silver Chloride. You said how you converted the Silver nitrate to Silver Chloride but nothing about reducing the Silver Chloride. If it did not melt into a metallic bar you likely never reduced the Silver Chloride to metal and actually melted the chloride into crumbly biscuits to use your description.

A few more details and we can likely help you fix this.

View attachment VID-20230720-WA0114.mp4

 

[Robson]

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View attachment 58184

View attachment 58184

 

[4metals]

Looks like Silver Chloride. Silver Chloride melts and boils but does not decompose without the proper fluxes. so if you didn’t reduce all or most of the chloride to metal your end result will be a melt of the combination of Silver metal and Silver Chloride. Likely the melt produced a white choking fume?

 

[4metals]

If you search the forum using “frying pan” you will find a post to use a frying pan (clean cast iron) sulfuric acid and the Silver Chloride you have crushed up into small pieces (powder is best).
Right now that’s your best option.

 

[Proffshuggarn]

Hi Robson
I hope you get that silver thing sorted out.
I just learned some basics with gold from e-scrap and actually managed to recover a few grams. So I thought that now I'm going to take a little "gold-break", while my stock pot is allowed to bubble and in the meantime I'll work on the silver I've accumulated, which I (as when I started with the gold) thought would be a "piece of cake".

But the more I studied and read other people's posts about the problems they encountered and the fact that I have not yet figured out how to solve the (as I understand it) extensive and prolonged stirring under continuous heat that is needed (veterans, please correct me if I have misunderstood the process), and without getting lye-splashes on me.
But I will negotiate with and justify to my wife why I have to buy a stirrer with an integrated heater .
Enough about that..

You seem to be on the right track anyway and I think you'll probably master it soon. Then feel free to teach me when I mess up with my silver process, because I WILL for sure .

But a little advice from a newbie like me: on your film, I recognize the color of your thumb nail.. Please use always gloves my friend. And all the protective equipment you have, which you probably already do.

I've also had everything from purple, yellow, blue spots on my hands and nails, which appeared when I "just" moved a couple of beakers or filtered.

Incidentally, I like your 10 pictures a little further back in the thread, very informative . Just kidding. Gets a little wrong sometimes, only human. Good luck now, you'll figure it out .
Best wishes
/Dennis

 

[user 72646]

Hellow My frends, i made a process with silver from contacts, in nitric acid, i preciptated with HCL, and a got a very strange result. i`ll be posting here the photos of something that looks more like a kind of crumbly biscuit, which after being melted does not react to acids agan. i really don`t know what it is, remembering that the silver also came ok.

Hi

did the crumbly stuff look like this?
It is grey White...the yellow is a filter bag
It came from a gold solution pre SBM.
Let me know your thoughts
Appreciated
M

 

[Yggdrasil]

Hi

did the crumbly stuff look like this?
It is grey White...the yellow is a filter bag
It came from a gold solution pre SBM.
Let me know your thoughts
Appreciated
M

He is/was refining Silver with Nitric.

You have given us little information that can help us help you.
How are you dissolving your Gold?


Anyway, welcome.

I want you to study this:

1. Read C.M. Hokes book on refining jewelers scrap, it gives an easy introduction to the most important chemistry regarding refining.
It is free here on the forum: Screen Readable Copy of Hoke's Book
2. Then read the safety section of the forum: Safety
3. And then read about "Dealing with waste" in the forum: Dealing with Waste

Suggested reading: The Library

https://goldrefiningforum.com/threads/gold-refining-forum-rules.31182/

Edited for spelling

 

[user 72646]

Hi

Thanks for the book "heads up".

I basically made an AP Vinegar and peroxide for some circuit boards fingers waited 4 weeks then filtered. I added some HCL then filtered again. The first filter without hcl produced a series of colours in respect to filtered material... This is pre SMB. I was going to add some Nitrate to the filtered solution, then attempt to drop the gold, if any exists. I ended up with a bunch of jars with multiple possibilities..
The Hcl made solutions go yellow prior to filter, some had white grey muddy stuff on base of jar and floating around?

I dried one piece, it is an odd thing to look at, as i have no idea what it could be...

Note
This is my first attempt at refining. i do not want to add any nitrates to these solutions, as i am yet to get my Stannous solution tested/working. Also i have little idea of the reaction that may occur.
Could you give me an idea of what these may be?

Appreciate the book!

MM

 

[user 72646]

THANKS FOR THE BOOK TIP
IT IS BRILLIANT...AFTER JUST 5 PAGES.. (silver section)

Thanks again
MM