Need Help - Iron - Silver Chloride

[Gemologist]

Ok new one here so be kind of nice to me.... I had a bunch of silver in my silver pot and added more when it started to dissolve to burn off the nitric acid. and noticed it turning a dark brown color.

So I then took out the silver and noticed several small magnetic pieces in the solution. So I tried to use more nitric acid and dissolve what I had and then was going to cement the silver out with copper and start all over. (please note there are no precious metals besides silver in solution.

Well when adding nitric acid by small amounts had a delayed reaction with a boil over (dark brown goop).

I took it off heat, let cool and added a bit more or nitric acid and the solution separated, dark green on top and dark brownish on the bottom.

siphoned off the green, left the brown, cemented the green with copper all seemed to be working ok, was thinking I saved it.

NOW THE ISSUE AT HAND

I added HCL to the brown liquid to see if there was silver in solution, not thinking as I should of only do this to a little bit of the solution. Well this is the problem. Obviously there was silver in solution, and now I have a mess with silver chloride. approx 1400ml. See photo.

What do I do now??

Thanks. Just want to get the silver out of solution but if I have to scrap the whole mess, that would be my lesson.

Thanks.

Mark

 

[Yggdrasil]

Ok new one here so be kind of nice to me.... I had a bunch of silver in my silver pot and added more when it started to dissolve to burn off the nitric acid. and noticed it turning a dark brown color.

So I then took out the silver and noticed several small magnetic pieces in the solution. So I tried to use more nitric acid and dissolve what I had and then was going to cement the silver out with copper and start all over. (please note there are no precious metals besides silver in solution.

Well when adding nitric acid by small amounts had a delayed reaction with a boil over (dark brown goop).

I took it off heat, let cool and added a bit more or nitric acid and the solution separated, dark green on top and dark brownish on the bottom.

siphoned off the green, left the brown, cemented the green with copper all seemed to be working ok, was thinking I saved it.

NOW THE ISSUE AT HAND

I added HCL to the brown liquid to see if there was silver in solution, not thinking as I should of only do this to a little bit of the solution. Well this is the problem. Obviously there was silver in solution, and now I have a mess with silver chloride. approx 1400ml. See photo.

What do I do now??

Thanks. Just want to get the silver out of solution but if I have to scrap the whole mess, that would be my lesson.

Thanks.

Mark

Welcome to us.

What have you done to the green liquid?
The brown was obviously not treated ideally.
Just make sure you have converted all the Silver to Chloride.
Then wash/boil it in HCl as it will do nothing to the Silver Chloride.
Repeat this until your Silver Chloride is clean and white.
Then convert it to Silver with either the Lye Sugar method or Acid Iron/Zinc method.
If you want you then run it through a Silver cell or refine it chemically again.

Here is some good links to study to help avoid some mistakes in the future:

We ask our new members to do 3 things.
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: https://goldrefiningforum.com/phpBB3/viewtopic.php?f=54&t=19798
2. Then read the safety section of the forum: https://goldrefiningforum.com/forums/safety.47/
3. And then read about "Dealing with waste" in the forum: https://goldrefiningforum.com/threads/dealing-with-waste.10539/

Suggested reading:
https://goldrefiningforum.com/forums/the-library.101/
https://goldrefiningforum.com/threads/when-in-doubt-cement-it-out.30236/
https://goldrefiningforum.com/threa...le-read-this-before-you-post-about-ore.33333/


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

 

[anarxi]

Ok new one here so be kind of nice to me.... I had a bunch of silver in my silver pot and added more when it started to dissolve to burn off the nitric acid. and noticed it turning a dark brown color.

So I then took out the silver and noticed several small magnetic pieces in the solution. So I tried to use more nitric acid and dissolve what I had and then was going to cement the silver out with copper and start all over. (please note there are no precious metals besides silver in solution.

Well when adding nitric acid by small amounts had a delayed reaction with a boil over (dark brown goop).

I took it off heat, let cool and added a bit more or nitric acid and the solution separated, dark green on top and dark brownish on the bottom.

siphoned off the green, left the brown, cemented the green with copper all seemed to be working ok, was thinking I saved it.

NOW THE ISSUE AT HAND

I added HCL to the brown liquid to see if there was silver in solution, not thinking as I should of only do this to a little bit of the solution. Well this is the problem. Obviously there was silver in solution, and now I have a mess with silver chloride. approx 1400ml. See photo.

What do I do now??

Thanks. Just want to get the silver out of solution but if I have to scrap the whole mess, that would be my lesson.

Thanks.

Mark

By adding hydrochloric acid you made aqua regia, which finally dissolved the iron.
The absence of a fox's tail or red hair does not mean that all of the nitric acid has been exhausted.
let the solution settle, time and gravity will do their job, the chloride will collect at the bottom.
Carefully decant the liquid and fill with clean, always hot (90 -95 degrees) water.
the chloride clumps, decant the water again, pour in diluted hydrochloric acid and wait an hour, the chloride will again disintegrate into sand.
Repeat filling with hot water, the rinsing water will be clean.
reduce the chloride to silver, since you have hydrochloric acid, you can reduce it with aluminum.