Tried my hand at silver. I've clearly made a mistake.

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Worms4u

Member
Joined
Dec 6, 2016
Messages
14
I like to give a detailed explanation so.. here goes.

I bought some silver plated silverware dirt cheap to try my hand at refining some silver. I ran it through a reverse electroplating cell and scraped off all of the silver, easy. Since I knew there was copper mixed in with the silver (Because the metal under was brass) I boiled the scrapings in HCL after washing the electrolyte off very well. After removing the copper I washed that very well too (No blue/green residue in the wash water when I was done - I used distilled water). So now I am left with a grayish kind of silvery material, it's kind of chalky. I was under the impression that this was elemental silver, and now I'd just dissolve it in Nitric/water and drop it out with some copper.

That's the problem - It's not happening. I've added water/Nitric and boiled it, it does nothing. Is this material a dirty AgCl? I thought it would be almost white if it was AgCl, but since it was gray/silvery that I assumed it was just Ag.

So my guess is that it's a chloride and I need to convert it to elemental silver, and then use nitric to refine it? It's not cottage cheesy though.. it's like a smooth chalky substance.

I'm kind of confused.

If it is AgCl, what would be the best way to convert it to elemental silver?
 
A foto would make it easier to understand.

Whatever you have Ag, AgCl or a blend of both, if it ist still wet, you can use NaOH or the NaOH/sugar-method to convert AgCl to Ag2O or elemental Ag and melt (Ag2O is turning to elemental Ag under heating).

If you have dried it (what you another time should avoid) you can smelt it with NaCO3, if I remember correctly. This method will cause some losses.

For detailed instruction, use the keywords I have given you with this post and try the search function. If you can't find it, ask again.
 
there is still copper in solution, wash until really clear, the test wash water for cobber, if you want to be sure
 
some prefer zinc, others prefer lye or lye and sugar, some even prefer to do it the hot way - that's up to you
 
Oh that was the picture I took when there was still nitric+water in the solution. Since it's AgCl I'll clean it real well and try zinc/fe + sulfuric - Because it was never really 'cheese curdy' so I don't know if the structure changed, and would have a problem with caustic soda.
 
Hi! So I converted everything to elemental silver, and wanted to chemically refine it (I'll try an electrolytic cell later). So I put my silver into 50/50 water/nitric acid and, the results were a little unexpected. There was a reaction, with the tell-tale red gas coming out of the beaker, but after heating the contents, and leaving it overnight here's what I am left with:

http://imgur.com/a/GPCLh

Note, I feel like I have used a lot of nitric acid. The contents does settle if left unheated. I kind of expected it to go completely into solution so I could drop it out with copper wire.

Do I need to add more nitric acid? I am pretty sure there is a little AgCl in it, but not a lot. I kind of figured I'd decant the silver nitrate out and then deal with the AgCl later.

Suggestions?
Thanks!
Worms
 
Worms4u said:
Hi! So I converted everything to elemental silver, and wanted to chemically refine it (I'll try an electrolytic cell later). So I put my silver into 50/50 water/nitric acid and, the results were a little unexpected. There was a reaction, with the tell-tale red gas coming out of the beaker, but after heating the contents, and leaving it overnight here's what I am left with:
what method did you use to convert?
http://imgur.com/a/GPCLh

Note, I feel like I have used a lot of nitric acid. The contents does settle if left unheated. I kind of expected it to go completely into solution so I could drop it out with copper wire.
1.22mL of acid per g of silver, same for water...less even if its pure and in a vessel with a watchglass
Do I need to add more nitric acid? I am pretty sure there is a little AgCl in it, but not a lot. I kind of figured I'd decant the silver nitrate out and then deal with the AgCl later.
Uhh, Id say no..you probably have ten times too much nitric in it already. Looks like silver chloride to me.
But, to know for sure. Set it in sunlight for a little bit. Does it turn black? If yes, then it needs converted to silver metal. ..

.But, with how you recovered the silver initially, it could be silver sulfate, or another metal from the base metal its plated on. Its really difficult to economically process silverplate stuff

Suggestions?
Thanks!
Worms
 
From what I can tell from the picture.

Should just try just a small amount of the powder in the test. The powder can be mostly other metals, nitric on the whole volume of powders to begin would just waste HNO3.

The red fume tells you that you have much of your nitric going up in gas, diluting the HNO3 and adding a little 3% H2O2 can help conserve your nitric and consume it in the reaction, it may take a little longer or heat but is not so wasteful or does not make such a deadly cloud.

Decant the solution you have now (test it for silver) using a copper wire or NaCl, black powder on copper, or white AgCl with the salt.

If the test above shows no silver do not get discouraged yet, the other metals may have replaced the nitric acid solution and cemented the silver back out with the rest of that volume of undissolved powders.

Do the test again with diluted Hno3 on a smaller volume, with just a spoon full or your powder, see how much dissolves, the color of solution , the volume of precipitate with salt (AgCl which is normally more voluminous than Ag cemented on copper), or the volume of Ag (black powder cemented with copper), compare that with volume of powders dissolved...
 
:D :( So, I finally said to heck with it and precipitated everything out as a chloride, so I knew what it all was. Then I stirred in some lye until it was black (or nearly so, very dark purple) And allowed the solution to cool and settle. So I've got silver oxide. At this point I could have melted it into elemental silver, but I though why not try this Karo method I've heard about. After watching a couple of videos I mixed in some Karo and I felt the solution heat up again. Then I come here and see the post "Do not use Dark Karo syrup", which is exactly what I did - Because that's what they used in the video!

Since it does not explain WHY you dont want to use dark karo syrup in the other post. Why not? Will it just be a sticky mess I'll have to dry out and purge with intense heat? Or is it simply not going to react and I have silver oxide still with some sticky stuff mixed in?

Due to the law of conservation I guess either way I can just fire and slag off the junk, I guess I just want to know why regular Karo is 'bad' and if it is, am I supposed to use the 'light karo'? Further if I am, why don't people specify light karo when they talk about it :(
 
Thanks Jimdoc, your reply was very enlightening, and useful. I am glad you took the time to post something so useful without addressing a single question I had! Look I can be snarky too!

I should mention I didn't go crazy with the dark karo syrup. I can use the light stuff to finish the reaction if needed.
 
If I had an answer for you, I would have given it.
I am not a Karo syrup expert. I do know not to trust Youtube videos though.
 
I think what Jim was trying to point out was the answer to your question is here on the forum, but that would take time and effort to find the answer. That's to hard compared to the easy way and instant gratification obtained from watching a youtube video. Now we are back to answering your question with our time and effort from a mistake you made there by lessening your burden and bestowing instant gratification to your situtation when all you had to do was follow this link: https://goldrefiningforum.com/phpBB3/search.php?keywords=
 
Worms4u,
I believe you owe Jimdoc an apology.

He was not being "snarky", he was trying to be helpful with his simple comment.

Maybe you are used to other forums or media on the web, things are much different here, that dog does not hunt here.

Here we are gentlemen and ladies which help each other in a professional manner, if not then they are politely asked to leave, or they are quickly shown the door.

You are very welcome here on the forum, if you can, and will conduct yourself as a gentleman, in a professional manner.

This is not the first time you have been warned, there will be no more.

I am no expert on Karo syrup they are both sugars and should work in the reaction.
Karo light corn syrup is made with corn syrup and real vanilla. Dark corn syrup is made with refiners' syrup, a type of molasses. could have something to do with its thickness or how it is made. I do not know, maybe someone who knows can answer the question, who has experienced the problem with it. If you will be polite.
It may just need to be diluted, I do not know and do not have time to experiment to find out.
 
butcher said:
Worms4u,
I believe you owe Jimdoc an apology.

Not expected, and not needed by me. If he does apologize, let it be to the forum with a promise to change his crappy attitude.

Looking back at his past attitude, I feel he should have been banned then.
And I can't really see him changing now. I predict he will be banned sometime in the future.

Here he is an accident waiting to happen, while chasing pennies worth of silver playing with chemicals he probably doesn't know about their hazards, or care about their safe disposal.

If he really wants some silver, he should buy it on Ebay.
 
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