silver chloride to silver metal MESS. need help.

Hello. I would like to get help fixing a mess i did trying to refine silver using silver cholride and NaOh. I have filtered siver cholride from nitric using salt. Washed well with distiled water. Next i have added NaOh and stirred until all powder was dark color. Next add caro (syrop) to try and get siver metal. Got the reaction and then some gray color powder. Washed well and dryed. Until now all was ok. When i have tryed melting it i have noticed that the powder dont melt but become black and red cherry color some silver did melt. Got lot of smoke. .
I think i have used more the i needed NaOh and caro.

How do i recover the silver back to a way i can rerefind it using the simple nitric copper way that had worked well for me in the past.

I did tryed to put some of the powder back in nitric. It disolved partly and now there is gery color powder that wont dissolve any more.

Thank you ( sorry for my poor english) .
Amit

I think you should keep using the search function.

How about this, skip the karo syrup nonsense and just use 5% dilute sulfuric acid and tumble your silver chloride in a plastic concrete mixer with steel balls or grease free iron punchings or even nails. Works great. Remove the magnetics with, guess what, a magnet, rinse off, take a test sample (please do that, so you don't repeat your previous problem of melting without incomplete conversion), and if it's good, go with it.

Lou

Thank you lou. I will do this next time. But can you tell me what is the powder i have now? And how can i save the silver?

Regards
Amit

Sounds to me like you didn't convert all your silver chloride to silver metal, there are several ways to convert it all of which are covered here on the forum in detail, as usual Lous suggestion is spot on and could be used to convert the rest of your silver chloride to metallic silver but there are other methods find the one that suits you.

Thank you all.
I will update the results.

Regards
Amit

Like Nick said, sounds like incomplete conversion. Especially if the silver chloride was dried out at the start, this could happen.

Maybe your math was wrong. It takes about 20g of NaOH and 13.3ml of light Karo per troy oz of silver (41.3g of AgCl). I like to use about 10% extra of each.

You also need lots of agitation when using the Karo. I like to use an old blender and let it run on low for an hour or more.

Amitoha23:

All what Lou,Nickvc,GSP and Rickbb have said to you is perfectly right.I agree with them,incomplete conversion of silver chloride is your problem.

Silver chloride contamination could be responsible of that incomplete conversion.Keep in mind that silver chloride must be washed with tap water many times and the last one must be done with hot water.As a rule of thumb,silver chloride is well washed if it is completly white and wash water is almost clear,any other condition will lead you to incomplete conversion.

Anyway,you have come here to find answers...What to do with that mess of silver/silver oxide and silver chloride you have?Well,in my personal opinion you should use Na2CO3(sodium carbonate) process,wich consists in:

-Weight the mess
-Grind it as fine as possible
-Add its same weight of Na2CO3
-Mix the mixure welll
-Heat mixure to 350-400 C,as a rule of thumb a solid chemical reaction will form a crust on top´s mixure,it means that silver chloride has converted into metallic silver,so break the crust and mix well and continue formig a crust until all the mixure has converted into a crust.
-Now rise temperature to 1100 C and you will see that little white balls of silver are formed,add some borax to collect them,pour off the flux and you will get a nice white ingot of silver.

I hope it helps.

Kindest regards.

Manuel

Manuel, I knew about sodium carbonate from Lou post http://goldrefiningforum.com/phpBB3/viewtopic.php?f=50&t=3264&p=32670#p32670 to go from silver nitrate to metal. So, are you mixing silver chloride in some water (probably tap water) and add sodium carbonate or do you mean to do all this dry.

I'm asking because I've saved some silver chloride under water (but light turned it dark) and when time arrives I thought to add NaOH, wash well, nitric leach, decant and siphon the leach from any unconverted AgCl and reduce it with sodium carbonate (wondering if bicarbonate would be also be ok).

It's a cocktail of two processes, hoping I got this right...

Marco

I don't think you should mix processes, chose one that you are comfortable using.

Personally would use the lye/sugar method. But that's the one that I've used more often and know what to expect from it.

Edit to add:

You can't use bicarbonate directly, but bicarbonate can be made into sodium carbonate by boiling off the CO2 and water. Heat it dry in an oven or in a fry pan on a stove at high heat until it no longer "steams" off the water and CO2. Takes about 20 to 30 minutes to complete.

DANGER! do this outside on in well ventilated place. It's only dangerous as it releases CO2 and replaces oxygen. Don't want to do that in a closed space like a small kitchen.

Good point about closed areas.

I remembered CO2 is heavier than air, so if a toddler, or pet, got into a lower area, they could suffocate. Please use caution for those you love.

Update. I have implemented Lou`s advice using sulfuric and iron (nails) worked perfect. Here the finel product(3oz) :


Thank you all for your help. Every time i learn somthing new.

Amit

You'll never go wrong by following Lou's advice. 8)

Dave

From Lou's "nonsense" comment and Amit's result I'm now convinced how to process silver chloride!

MarcoP said:

From Lou's "nonsense" comment and Amit's result I'm now convinced how to process silver chloride!

Click to expand...

Lazersteve has a free video on his site that shows the process with sulfuric and steel.

Thanks Geo, I've watched many of Steve's video and read his PDFs and even this time I'll have to wait to watch the video for when I go back home, probably a week or so. Time it's not an issue anyway hehe... thanks again.

Converted many thousands of ounces that way.

amitoha23 said:

Hello. I would like to get help fixing a mess i did trying to refine silver using silver cholride and NaOh. I have filtered siver cholride from nitric using salt. Washed well with distiled water. Next i have added NaOh and stirred until all powder was dark color. Next add caro (syrop) to try and get siver metal. Got the reaction and then some gray color powder. Washed well and dryed. Until now all was ok. When i have tryed melting it i have noticed that the powder dont melt but become black and red cherry color some silver did melt. Got lot of smoke. .

Amit

Click to expand...

Hello,

You don't need to use distilled water to wash the silver powder or the silver chloride, tap water works fine for both.

I had this happen to me once. I did not get all the lye washed out before I dried and then melted the silver.

The melted silver had a horrible red color to it.

The lye etched a Corning ware dish that I used to dry the silver powder.

When washing the lye and sugar from your silver, do pH tests with tests tips to make sure you are all the way neutral with pH of 7 before you commit to drying and melting.

I have seen the pH get to 6 (slightly acidic) with test strips during my washes with tap water.

How the pH got to 6 I'll never know, but with the pH at 6 (six) I was absolutely certain that all the lye and sugar was gone from my silver.

Using tests strips to test pH when washing the silver, I have never had this problem again.

kadriver

Lou said:

How about this, skip the karo syrup nonsense and just use 5% dilute sulfuric acid and tumble your silver chloride in a plastic concrete mixer with steel balls or grease free iron punchings or even nails. Works great. Remove the magnetics with, guess what, a magnet, rinse off, take a test sample (please do that, so you don't repeat your previous problem of melting without incomplete conversion), and if it's good, go with it.

Click to expand...

I did this, and it works like a charm! And a lot quicker and less messy than cementing.

Anyway, it occured to me that the leftover solution could be a weak Iron Sulfate (copperas) solution. I have more copperas than I need at the moment, but could this solution be concentrated/evaporated and used to precipitate gold? Perhaps for a first drop, then a second refine using SMB?

Edit: I've also seen it mentioned to store your copperas with a drop of sulfuric acid to keep it fresh. Another possible use for this waste liquid? Otherwise, I'll just keep using this solution for the tumbling process until it fails to work any more.