I tried converting washed and cleaned silver chloride to metallic silver using the sugar and lye method and it clearly didn't go well. Trying to see if anyone can help me fix this issue. After using the sugar and lye method, I washed the precipitate, then tried melting it, in which some parts of the precipitate melted into silver buttons, while other parts were just a crumbled unmelted mess (there was a mixture of both crumbled unmelted pieces and fully melted silver in the crucible). What should I do with the parts that did not convert into metallic silver? Can I recover from this and start over? In the pictures showing the corningware dish, the precipitate pieces on the left are after trying to melt (which resulted in the mixture of both crumbled unmelted pieces and fully melted silver in the crucible), while the precipitate pieces on the right have not been melted yet.
Silver chloride conversion issues
- Thread starter icejj
- Start date
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Do you mean Lye first then Sugar or as you are saying above sugar and lye?
Was the first step after wash Lye additions until the material was almost black like oxide and lots of stirring.
As you are stirring, stir some stuff to the glass side to see if there is a white smear.
If there is a white smear stir and add more lye until no white smear or line appears on glass. Stirring, stirring.
I use a battery drill with stir rod, or lots of hand stirring.
Then add sugar carefully stirring stirring I use KAO syrup carefully because it will react and keep heating up.
It can boil over like crazy. You will see the condensation on the beaker from exothermic reaction
Carefully I get to a near boil, also the color of the material is turning much lighter.
Use a casserole dish under the beaker just in case.
Pay attention to the proper colors.
I have a hard time telling with your pictures if you had enough heat when melting.
Was the first step after wash Lye additions until the material was almost black like oxide and lots of stirring.
As you are stirring, stir some stuff to the glass side to see if there is a white smear.
If there is a white smear stir and add more lye until no white smear or line appears on glass. Stirring, stirring.
I use a battery drill with stir rod, or lots of hand stirring.
Then add sugar carefully stirring stirring I use KAO syrup carefully because it will react and keep heating up.
It can boil over like crazy. You will see the condensation on the beaker from exothermic reaction
Carefully I get to a near boil, also the color of the material is turning much lighter.
Use a casserole dish under the beaker just in case.
Pay attention to the proper colors.
I have a hard time telling with your pictures if you had enough heat when melting.
I added lye first, then sugar. Yes, I added lye until almost black and did the smear test. I believe that I did all of the steps that you mentioned correctly, but based on my results it seems as if I was wrong somewhere. I believe I had enough heat, as some parts were completely melted and flowing while other parts was more of a soft crumbling substance until it hardened after removing the heat. I'll put the torch to it again tomorrow just to make sure though.
You did not convert all the Chloride to metal, that would be my guess.
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Any idea on how to proceed from here to convert the chloride to metal? Is this process different since now I have dried silver chloride and maybe something else????
I guess smelting is the only option now.
Thank you. I will read more on this and give it a try!!!
I would start dissolving everything again.
Rinse the “vinaigrette” with hot distilled water and decant several times.
Then fill everything with nitrogen and boil a little, stirring.
Some of the reduced chloride will dissolve.
Then I would drain the acid through a filter and work with it through chloride, only reducing it with aluminum and hydrochloric acid.
I would fill the precipitate undissolved in nitric acid with the first water that remained after converting the nitric solution into chloride + hydrochloric acid.
I would throw aluminum there and try to restore this sediment, which turned into chloride..
washing again, bringing the psh to neutral and again nitric acid...
Silver chloride will melt and remain as silver chloride at a lower temperature than the Silver metal melts. It indicates two things, one, the conversion to Silver metal was incomplete, and two the melt was not a homogenous mix so the chlorides melted but they all did not get hot enough to reduce to metal.
Silver Chloride that has been melted can be poured and it will appear to be slag like and brittle.
The chlorides can be tumbled in a 10% sulfuric acid solution with a few iron nails. As the iron contacts the chlorides they will reduce to metallic Silver.
Silver Chloride that has been melted can be poured and it will appear to be slag like and brittle.
The chlorides can be tumbled in a 10% sulfuric acid solution with a few iron nails. As the iron contacts the chlorides they will reduce to metallic Silver.
It looks like you didn’t add enough lye while stirring then went on add sugar without it being fully converted.
Based on your crucible picture. You’re burning the chlorine and sugar/lye combination because it’s not been converted to an oxide fully. The black carbon and slag is a clear indicator.
It also happens most noticeable when you don’t wash your chloride enough. It could have other contaminants in the chloride. All depends what other base metals are possibly present.
HCL precipitation will also drop for instance lead chloride as well. If present in the solution.
Visual indicators are when you have the silver melted. Youll create a crazy slag from the hydroxide and sugar combo because it melts at a much lower temperature then silver. If you pour it into a mold the silver will drop and the lye/sugar/chlorine will sit on top of the silver in the molten state.
When you pour it. The slag will lock you bars in the mold. Pain the the rear to get them out.
My suggestions:
would be to invest in an electric drill. You can buy chemistry stirring rods that are acid proof. PTFE material.
Buy a PTFE 5 gallon bucket. Home Depot/Lowes/Amazon.
When adding lye. Dissolve more the enough in water. It doesn’t have to distilled water at this point. Once all the hydroxide is dissolved in the water pour it into the chloride while aggressively stirring. Minimum of 10 minutes of stirring. Until you visual see all the white
gone or all the silver converted to Ag2O. (black oxide).
Once it’s all converted. Keep the lye solution stirring while adding granulated sugar. This will cause a massive thermal reaction. Slow pour sugar until the solution stops boiling or reactive to the sugar additions.
This whole describing process shouldn’t take more the 10-15 if your prepared before hand.
My opinion you can’t really add to much lye so don’t worry on that end. I also never add so much to test this theory.
You can 100% add to much sugar which creates molasses. Pain to get it out of the silver.
Hopefully this helps!
Based on your crucible picture. You’re burning the chlorine and sugar/lye combination because it’s not been converted to an oxide fully. The black carbon and slag is a clear indicator.
It also happens most noticeable when you don’t wash your chloride enough. It could have other contaminants in the chloride. All depends what other base metals are possibly present.
HCL precipitation will also drop for instance lead chloride as well. If present in the solution.
Visual indicators are when you have the silver melted. Youll create a crazy slag from the hydroxide and sugar combo because it melts at a much lower temperature then silver. If you pour it into a mold the silver will drop and the lye/sugar/chlorine will sit on top of the silver in the molten state.
When you pour it. The slag will lock you bars in the mold. Pain the the rear to get them out.
My suggestions:
would be to invest in an electric drill. You can buy chemistry stirring rods that are acid proof. PTFE material.
Buy a PTFE 5 gallon bucket. Home Depot/Lowes/Amazon.
When adding lye. Dissolve more the enough in water. It doesn’t have to distilled water at this point. Once all the hydroxide is dissolved in the water pour it into the chloride while aggressively stirring. Minimum of 10 minutes of stirring. Until you visual see all the white
gone or all the silver converted to Ag2O. (black oxide).
Once it’s all converted. Keep the lye solution stirring while adding granulated sugar. This will cause a massive thermal reaction. Slow pour sugar until the solution stops boiling or reactive to the sugar additions.
This whole describing process shouldn’t take more the 10-15 if your prepared before hand.
My opinion you can’t really add to much lye so don’t worry on that end. I also never add so much to test this theory.
You can 100% add to much sugar which creates molasses. Pain to get it out of the silver.
Hopefully this helps!
kurtak
Well-known member
My first question is what was the original source from which the silver chloride came ?
in other words - did you dissolve sterling silver - or contact points - or something else (like solder etc. etc.) in nitric & then use salt or HCl to drop silver from nitrate solution as silver chloride
I ask because depending on what the original source of metal was &/or how or when the "white" precipitate was produced could determine if it is silver chloride contaminated with other base metal salts (such as lead chloride or copper oxides etc.) or if it is even silver chloride at all
I ask the last part of that question because you make no mention about the salt (HCl) of the salt/lye/sugar part of the silver chloride process - you only mention the lye/sugar part
In other words - are you trying to convert "some other" white precipitate that came from some other process - such as a white precipitate that came from an AR process &/or even a white precipitate that formed "during" a nitrate process with no salt added to form the precipitate
second question - did you let the silver chloride dry out ? (assuming it is/was actually silver chloride dropped with salt/HCl from a silver nitrate solution)
I ask because when I look at the picture of the jar it looks like a white precipitate that has been dried out (chunks instead of a wet precipitate that is well settled by being kept wet)
Silver chloride - once it has dried out - does not respond well to the lye/sugar part of the conversion process - even if/once you re-wet it
In other words - you will not get complete conversion of the silver chloride to silver oxide with the lye - which in turn means that you wont get complete conversion to actual silver with the sugar part of the process --- even if you crush the dried out silver chloride to a fine powder
So please answer both of those questions so that we can get to the bottom of solving your problem
Then also - when looking at your pictures of your attempts of melting I see a LOT of black residue which is likely the result of ------------
1) base metal oxides being formed due to base metal contamination (as explained in my first question)
2) carbon being formed as a result of not washing all the sugar out after the sugar part of the process
3) a combination of the above two
Kurt
in other words - did you dissolve sterling silver - or contact points - or something else (like solder etc. etc.) in nitric & then use salt or HCl to drop silver from nitrate solution as silver chloride
I ask because depending on what the original source of metal was &/or how or when the "white" precipitate was produced could determine if it is silver chloride contaminated with other base metal salts (such as lead chloride or copper oxides etc.) or if it is even silver chloride at all
I ask the last part of that question because you make no mention about the salt (HCl) of the salt/lye/sugar part of the silver chloride process - you only mention the lye/sugar part
In other words - are you trying to convert "some other" white precipitate that came from some other process - such as a white precipitate that came from an AR process &/or even a white precipitate that formed "during" a nitrate process with no salt added to form the precipitate
second question - did you let the silver chloride dry out ? (assuming it is/was actually silver chloride dropped with salt/HCl from a silver nitrate solution)
I ask because when I look at the picture of the jar it looks like a white precipitate that has been dried out (chunks instead of a wet precipitate that is well settled by being kept wet)
Silver chloride - once it has dried out - does not respond well to the lye/sugar part of the conversion process - even if/once you re-wet it
In other words - you will not get complete conversion of the silver chloride to silver oxide with the lye - which in turn means that you wont get complete conversion to actual silver with the sugar part of the process --- even if you crush the dried out silver chloride to a fine powder
So please answer both of those questions so that we can get to the bottom of solving your problem
Then also - when looking at your pictures of your attempts of melting I see a LOT of black residue which is likely the result of ------------
1) base metal oxides being formed due to base metal contamination (as explained in my first question)
2) carbon being formed as a result of not washing all the sugar out after the sugar part of the process
3) a combination of the above two
Kurt
If I understand it correctly.
The pictures is from after trying to melt the "converted" Silver.
This ended up in some Silver buttons and what we see in the pictures.
Which means the wet conversion route is closed.
kurtak
Well-known member
Per the bold print first quote - so he has not tried to melt all of it yet
Kurt
Strange, to me they looks like solid Silver in the picture.
Lets wait for Icejj to chime in.
