Silver from Litho film fix

[joem]

hello
does anyone know of a retail chemical to precipitate silver from litho film fix? I tried baking soda, soda ash, aluminum foil, steel wool but it just leaves a lot of rust behind, electroplate but I can't seem to get the current right (SS and carbon, SS and Copper, SS and Aluminum) no effect.
sodium sulfide, sodium borohydride or sodium dithionite are not available to me, so I'm asking about your experience.
thanks
joe

 

[Geld Konig]

Once I used Na2S and silver go to the botton like Ag2S. Let few day to precipitate the silver.Try to heat the solution in becker. After this, I filtrate the solution and take the precipitate -Ag2S - put into a baker and add HNO3 concentrate. You can heat the becker but take care to not overflow the solution. Filtrate the solution and add HCl or NaCl to form AgCl ( a white cloud that will precipitate with the time (let it a overnight to precipitate all AgCl.). Add more NaCl or HCl to know if all AgNO3 (solution) react and in the solution is not any silver.

 

[Juan Manuel Arcos Frank]

Joem:

- "THERE ARE MANY WAYS TO SKIN THE CAT"- (said by The Great Master,GSP)

You can use hypochlorite,NaOH,FeCl3 or oxalic acid processes...just use the search box.

Regards.

Manuel

 

[butcher]

Good place to put in a plug for GSP'S great book on silver, well worth the price for all of that invaluble knowledge he has acummilated, over the years as a proffesional silver refiner, and put into a book. better get one if he still has them.

 

[Lino1406]

NaOH powder, mix well.
Formalin will augment efficiency somewhat

 

[joem]

All in the name of all that is science
just don't tell my wife about my experiments
I added 1 cup of clorox bleach to two cups of litho silver film fix
here is what happened...

instantly turned brown and an increased in temperature - but a little
I let sit outside for a while and it turned coffee with lots of cream colour
there is about a 1/4 inch of fine brown powder at the bottom.

What's your thoughts on this?
joe

 

[Juan Manuel Arcos Frank]

It could be many things.Since my english is not good enough I understood you wanted to recover silver from litho films...so I was wrong.You can recover silver from litho fix adding sodium sulphide and then refine silver sulphide with a method I have posted here.Also,you can use zinc/sulphuric acid method.You need to know how to measure silver content on your fix and how to refine silver...here are some articles written by me,but,sorry...they are in spanish.I promise to write them in english ASAP.

I hope they help you to recover your silver.

Best regards.

Manuel

 

[joem]

Ok I went back to my original plan of getting silver from Litho film.
Found some Naoh at one location in the city.
Put 1/2 litre of film fix in a jar and added two table spoon size scooped,
stirred until dissolved and it instantly turned black.

Then I found this info on another site, does it have merrit?

"To convert silver chlorides to metallic silver you will need to use dry caustic soda (sodium hydroxide)and dextrose (corn syrup can be used).
Rinse the silver chlorides well with water to remove any residual copper. Place the wet silver chloride sludge in a suitable container 1/3 silver chloride with about 2/3 free board. leave about 4 cm of water on top of the silver chloride. Slowly add the dry sodium hydroxide a scoop at a time, stirring well. The reaction is exothermic as the silver chloride is converted to silver oxide. Some people like to add the dextrose along with the sodium hydroxide as it has a deflocing effect on the silver chloride. The dextrose converts the silver oxide to a metallic form. The dextrose can be added a scoop at a time after the sodium hydroxide has reacted with the silver chlorides. When no more reactions with the sodium hydroxide or dextrose occur the process is complete. The resulting silver is rinsed well, dried and melted. The purity of the silver will be 98% to 99% pure and electrolytic refining should be done for optimum purity. For rough calculations by volume of silver chloride - liters of silver chloride X .30 kilos sodium hydroxide - liters of silver chloride X .15 kilos dextrose"

 

[Oz]

The silver oxide you will get is rather clean using NaOH. I would just wash it with water, dry, and melt. Silver oxide decomposes (turns to silver metal) loosing the oxygen at a bit under 300C. Your molten bars should be as pure as cement silver.

 

[rusty]

It could be many things.Since my english is not good enough I understood you wanted to recover silver from litho films...so I was wrong.You can recover silver from litho fix adding sodium sulphide and then refine silver sulphide with a method I have posted here.Also,you can use zinc/sulphuric acid method.You need to know how to measure silver content on your fix and how to refine silver...here are some articles written by me,but,sorry...they are in spanish.I promise to write them in english ASAP.

I hope they help you to recover your silver.

Best regards.

Manuel

Manuel you may want to touch up on the Bablefish translation then repost the files.

 

[goldsilverpro]

Ok I went back to my original plan of getting silver from Litho film.
Found some Naoh at one location in the city.
Put 1/2 litre of film fix in a jar and added two table spoon size scooped,
stirred until dissolved and it instantly turned black.

Then I found this info on another site, does it have merrit?

"To convert silver chlorides to metallic silver you will need to use dry caustic soda (sodium hydroxide)and dextrose (corn syrup can be used).
Rinse the silver chlorides well with water to remove any residual copper. Place the wet silver chloride sludge in a suitable container 1/3 silver chloride with about 2/3 free board. leave about 4 cm of water on top of the silver chloride. Slowly add the dry sodium hydroxide a scoop at a time, stirring well. The reaction is exothermic as the silver chloride is converted to silver oxide. Some people like to add the dextrose along with the sodium hydroxide as it has a deflocing effect on the silver chloride. The dextrose converts the silver oxide to a metallic form. The dextrose can be added a scoop at a time after the sodium hydroxide has reacted with the silver chlorides. When no more reactions with the sodium hydroxide or dextrose occur the process is complete. The resulting silver is rinsed well, dried and melted. The purity of the silver will be 98% to 99% pure and electrolytic refining should be done for optimum purity. For rough calculations by volume of silver chloride - liters of silver chloride X .30 kilos sodium hydroxide - liters of silver chloride X .15 kilos dextrose"

This is fine except you don't have silver chloride to start with. You have a more complicated silver thiosulfate complex and I don't know what the actual reaction products are when the NaOH was added. Chemically, though, I can't see how silver oxide was produced but I could be wrong. Maybe the NaOH broke down the thiosulfate and now you have silver sulfide. Manuel probably knows since he mentioned NaOH in his post above, although I didn't see it in his 3 articles. Whatever, don't add it to any more silver solution until you have proven that you can recover the silver from the 1/2 liter you have already treated. Keep in mind that you don't know if all of the silver is in the black sludge. Some may still be in solution - use Manuel's copper wire technique in his 1st article to check it.

 

[goldsilverpro]

I just searched the internet and got an education.

According to the attachment, sodium hydroxide (NaOH) precipitates silver hydroxide (not silver oxide) sludge from bleach-fix. The guy was able to ppt 96% of the silver by adding NaOH to a pH of 12. I think he says that further additions of NaOH did not improve on the 96% - that seems to be the recovery limit using this method. He also experimented with steel wool and got 99+%. However, separating the silver from the excess steel wool requires a crucible furnace and some know-how. If you don't have these, I would try to do it chemically.

So now you have this voluminous (probably) silver hydroxide sludge. What do you do with it now? No matter what you do, I would think that it would be necessary to first clean the sludge by filtering and rinsing it very well, since the presence of the chemicals in the fixer might (very possibly) cause problems down the line. This may be easier said than done, since most metal hydroxides are notoriously difficult and slow to filter and rinse.

According to this, silver hydroxide will decompose to metal at only 80C (176F), whereas silver oxide decomposes at 200C (392F). After cleaning the sludge, this may be as simple as just heating up a suspension of the sludge in water to a little below boiling. It would surely be worth a try.
http://silversol.net63.net/theory/cstheory.htm

After cleaning the sludge, you could dissolve it in nitric and then either cement the silver with copper or precipitate silver chloride and then reduce it to metal with one of several different methods.

A sugar, such as Karo syrup, would probably reduce the silver hydroxide to silver metal.

Play with it until you get a workable method.

 

[joem]

so now I have about 1/2 an inch of (according to chavalit's paper) silver hydroxide at the bottom of the liquid filled jar.
How would I go about using corn syrup to reduce to metal (silver oxide)?
And what are the issues with the leftover mix of fix solution and lye?
edit for leftover mix spelling

 

[joem]

so just a bit more information about the fix I'm am trying to recover silver from
two main ingredients
ammonium Thiosulphate
water
lesser equal parts of
Sodium Sulphite
Acetic acid
sodium acetate

 

[goldsilverpro]

so now I have about 1/2 an inch of (according to chavalit's paper) silver hydroxide at the bottom of the liquid filled jar.
How would I go about using corn syrup to reduce to metal (silver oxide)?
And what are the issues with the ledtover mix of fix solution and lye?

I was only passing on what I found on the internet. Since I haven't worked with silver hydroxide before, I would assume that Karo syrup would reduce it just as with silver oxide. With silver oxide, it takes about 13.3 ml of Karo syrup to reduce 1 oz of silver. You'll just have to play with it.

 

[joem]

so now I have about 1/2 an inch of (according to chavalit's paper) silver hydroxide at the bottom of the liquid filled jar.
How would I go about using corn syrup to reduce to metal (silver oxide)?
And what are the issues with the ledtover mix of fix solution and lye?

I was only passing on what I found on the internet. Since I haven't worked with silver hydroxide before, I would assume that Karo syrup would reduce it just as with silver oxide. With silver oxide, it takes about 13.3 ml of Karo syrup to reduce 1 oz of silver. You'll just have to play with it.

my question is how do I do that? Do I add an amount of corn syrup to the sludge and stir? Then see what happens.

 

[goldsilverpro]

so now I have about 1/2 an inch of (according to chavalit's paper) silver hydroxide at the bottom of the liquid filled jar.
How would I go about using corn syrup to reduce to metal (silver oxide)?
And what are the issues with the ledtover mix of fix solution and lye?

I was only passing on what I found on the internet. Since I haven't worked with silver hydroxide before, I would assume that Karo syrup would reduce it just as with silver oxide. With silver oxide, it takes about 13.3 ml of Karo syrup to reduce 1 oz of silver. You'll just have to play with it.

my question is how do I do that? Do I add an amount of corn syrup to the sludge and stir? Then see what happens.

I would add some water to it and stir it while adding the Karo. Try just a little bit of the sludge and see what happens. When you add the Karo, if it works the same as silver oxide, it will change to a gray, grainy silver, similar in appearance to cemented silver. I don't think it will hurt to have an excess of water or Karo.

To get an idea of how much water to use, when I did silver chloride, besides the NaOH and Karo, I used about 100 ml of water for each ounce of silver.

Like I said, play with it. I'm not sure it will even work.

 

[joem]

thanks gsp
I'll try it this weekend

 

[Anonymous]

hello
does anyone know of a retail chemical to precipitate silver from litho film fix? I tried baking soda, soda ash, aluminum foil, steel wool but it just leaves a lot of rust behind, electroplate but I can't seem to get the current right (SS and carbon, SS and Copper, SS and Aluminum) no effect.
sodium sulfide, sodium borohydride or sodium dithionite are not available to me, so I'm asking about your experience.
thanks
joe

You can precipitate the silver out with zinc dust; mix it well; let it settle; dry out the mud and fire it. Its easier to get a silver recovery unit from my friend Paul Hess of Rotex Corp. in Ohio. costs a couple of hundred bucks for a small unit and will plate out nice silver. Tell him Shelly from Chgo. referred you.

 

[joem]

thanks precious
does he have a web site?

edit: Is zinc powder the same as zinc oxide powder used for "baby Powders"