Recycling Silver

kq6up · May 3, 2011

I am interested in getting started with the wet plate process, and I have been experimenting with reclaiming the silver from my old fixer. I used electrolysis today, and almost instantly got a ton of black sludge. I would imagine this is atomic silver. I guess it could also be silver oxide. Either way I was planning on dissolving it into concentrated nitric acid to get AgNO3 to try with wet plate. I was also thinking about firing it in a crucible to see the shiny silver just for fun. Anyone have experience with using reclaimed Silver to make AgNO3. I am a HS Chemistry teacher, and I have access to a fume hood and all of the HNO3 I need.

Regards,
Chris Maness

alexhill · May 4, 2011

This is an antiquted but interested read. Start on page 1 (just kidding!) page 376 Instruction in Photography

kq6up · May 4, 2011

alexhill said:
This is an antiquted but interested read. Start on page 1 (just kidding!) page 376 Instruction in Photography

Thanks Alex. This is awesome. I tested my black sludge today in the lab, and yes -- it is Ag!

I was already planing on firing it in a crucible when I get enough separated out. It is good to see some info here (ancient as it is).

Chris

nhemann · May 4, 2011

How 'bout we agree to leave the opining and personal insults off the thread, eh? I can find enough of this poo elsewhere.

kq6up · May 4, 2011

nhemann said:
How 'bout we agree to leave the opining and personal insults off the thread, eh? I can find enough of this poo elsewhere.

I can agree to that. I was wondering if I should even dignify the above post with a retort. I felt obligated to let him know that these types of post are a TURN OFF to APUG, and the podspace/blogsphere warn neophytes to steer clear of APUG just for that reason -- because they will get blasted if they show any lack of knowledge.

My admonition for Jim to find happiness in his life is not tongue and cheek. I really mean it.

Chris

removed account4 · May 4, 2011

whether you are a chemistry teacher or an expert with years of experience making silver nitrate it doesn't really matter ...
it is dangerous, very dangerous ...

maybe you should add this to your list of things to read as well ...

Dead Link Removed

i know of people that used to make it, and sell it to folks in the alt-photo crowd but
they decided after a number of years it wasn't worth the danger ... ( of an accidental explosion )

bblhed · May 4, 2011

I would like to say that knowing how to do something, but checking that you are in fact doing it right, or seeing if someone else knows a better, safer, or quicker way of doing it should always be commended, not admonished.

What I was hoping to learn from this thread is at what point in the process if any do you have to work in the dark, I assume this has to happen at some point.

kq6up · May 4, 2011

Thanks for the support guys. I do wish to do it as safely as I can muster. I know the dangers of HNO3, if there is other issues with AgNO3 please post it here.

@jnanian I will read the thread.

Regards,
Chris Maness

railwayman3 · May 4, 2011

jnanian said:
i know of people that used to make it, and sell it to folks in the alt-photo crowd but
they decided after a number of years it wasn't worth the danger ... ( of an accidental explosion )

Maybe the OP would be best in selling his recovered silver compounds to a recycler.

I understood, on the Ilford factory tour, that they buy all their silver supplies in nitrate form, rather than as the basic metal, and that all silver waste is sent for recycling (even the bits punched to make the perfs of 35mm film ).

removed account4 · May 4, 2011

nhemann · May 4, 2011

Hazah! I did some serious learning with those articles (not that the thought to do that ever crossed my mind.) Unfortunately I am probably on an FBI watch list now just for reading those articles.

bblhed · May 4, 2011

Um, I think I will just buy Silver Nitrate in already made form, I have enough things to worry about.

kq6up · May 4, 2011

I read the thread. It is not explosive per the hazardous materials warning. It is a strong oxidizer so it needs to be stored away from combustibles.

Note taken on NO2. I was not aware that you could die three days later from edema. That was a new one for me. However, I conveniently have a lot of HNO3 at my disposal and a VERY nice fume hood. I will be mixing this behind glass. If the power fails while mixing, I will be getting out of dodge ;o)

The nice thing about NO2 is that it has a VERY pungent smell, and you will know if you are in a cloud of it.

Regards,
Chris Maness

greybeard · May 4, 2011

I have used the zinc dust cementation method, and found that a fraction of the residue was not soluble in nitric acid. Poking around in the precious metals reclamation literature revealed that silver sulfide is not soluble in nitric acid, and the preferred method for reclaiming it is to fuse with potassium nitrate. The resulting metal, of course, would be easily converted to nitrate. Any silver oxide originally present would decompose to metal during the fusion process. Have to try this one of these days......

removed account4 · May 4, 2011

kq6up · May 4, 2011

@greybeard. I am thinking what I had might have been Ag2S because very little of it dissolved in conc. HNO3. However, I started to add a few drops of HCl and ALL of it dissolved and formed the milky white precipitate that I am certain was AgCl. It had a yellowish cast that was due to the NO2 in solution. This cleared when I placed it in an evaporating tray in the fume hood.

When I gather enough of the dry black sludge. I am going to fire it in an iron (reducing) crucible with an Air-Acetylene torch. That should yield pure metallic Silver.

This is fun. I feel like an old timer )

Chris

alexhill · May 4, 2011

Gah!

Rather than all the 'herp/derp, you will die' posts, can we spend the time sharing helpful safety procedures? This reminds me of the KCN post I started..

I'm wicked jealous of you Chris. Any chance you are in New England?

Alex

kq6up · May 4, 2011

Nope, I am in Socal. Thanks again for the book link. That is the COOLEST thing I have seen. It is definitely before the don't poke your eye out days ;o)

Thanks,
Chris Maness

alexhill · May 4, 2011

I read that book front to back on my lunches, then came home to play. Its really awesome and super helpful (sometimes). My farmers reducer from it turned out a little strong and put some holes in my negative. I've got plans to try to make 'albumin' prints using frankincense instead of egg. It even has a diagram for a hydro powered tray agitator.

Good luck! Post a video of making it if you can.

P.s. you should try to manufacture uranium nitrate. It's ungodly expensive, and the coolest salt IMHO.

removed account4 · May 4, 2011

the reason there are a lot of "herp/derp you will die posts"
is because often times people who have no idea what they are doing
make their own silver nitrate or use cyanide &C thinking
everything is safe and dandy ...

if the OP didn't have a fume hood
he would probably be dead by now ...

alexhill · May 4, 2011

I think it's a lot more effective to describe the safe way to use something, and let people decide that its a bad idea, rather than deciding for them. If someone wants to do something, they will and you miss the opportunity to direct them in the right, helpful and safe direction.

And fume hoods are great! But most of us can't afford that kind of set up. Luckily my heros managed to get by without one, or even electricity for that matter.

mhcfires · May 4, 2011

Hmm*this post is beginning to sound like medieval alchemy.

kq6up · May 4, 2011

I did a separate test where I used hydrogen peroxide. I was thinking that it would oxidize the thiosulfate to a higher state, and percipitate the AgX out of solution. I got a precipitate alright, but it is either atomic silver or Ag2S. Strange and unexpected.

Chris

Mr Bill · May 4, 2011

kq6up said:
... I have been experimenting with reclaiming the silver from my old fixer. I used electrolysis today, and almost instantly got a ton of black sludge...

Chris, more than likely what you are getting is silver sulfide. This is the normal result of running too much current for the amount of silver available in the solution. Since, as you say, it happened almost instantly, my guess is that you are running way, way, way too much current, for the conditions.

So, what to do next? Did you rig up your own system (I'm guessing 'yes')? If so, how much current are you running? (If you don't know, and it is uncontrolled, this is most likely the problem). Next, how large is your cathode (and anode, too, while we're on the subject)? This will be in terms of surface area, square inches or the like. Lastly, are you circulating the fixer? Based on your answers, I can probably make some suggestions. Hopefully you still have some used fixer left to experiment with.

Maybe I should say that my purpose would be to get a good metallic silver plate on the cathode. If you're more interested in investigating things, or want to produce silver sulfide, that's fine too, refiners can work with that. But I don't think anyone would do that commercially, anymore. A well-controlled electroplating system can give you a known quantity, in the form of high-purity flake, so at least you have a very good idea of what's supposed to be there.

kq6up · May 4, 2011

@Mr. Bill

I had figured I went overboard with the current. I am going to try a variable pot with a light bulb for a load to protect the pot, and put an ammeter in line. I plan on using Aluminum for my next electrodes. The Ag is to make AgNO3 for wet plate process. I have plenty more fixer to play with.

Regards,
Chris Maness

Recycling Silver

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