Silver in NA, what did I do!

[PPDB]

Can anyone recognize what I’ve done here? And hopefully how to fix it.

This is my process w/ the things I believe I messed up in bold.

- Mixed 500ml nitric with 500ml water (Should have added nitric over time)
- Used a torch to heat up scrap and added it to the acid.
-I was outside in the sun.
-The hot silver reacted quickly
-One spoon had a stronger reaction than the others so I didn’t add its handle. The handle says ss but does not test for silver.
I then put the beaker on the hot plate. (High)
- The acid boiled down to 600ml so I added 400ml more water.
- Boiled until an added sterling spoon no longer reacted.
- As it cooled the purple/grey mud settled under a clear blue liquid.
-the mud cannot be filtered
-I added distilled water and let the mud settle so I could get all the blue liquid I could.

I used an oxy torch and melted some of the mud along with baking soda. I was able to cast a small bead of metal that is very brittle, not magnetic and below 80% silver. The bead reacts with nitric.

I diluted some mud with water and added some hcl. A white precipitate formed. I’m guessing this is some silver from the solution that is the liquid component making the mud.

So… that’s my mess. Thanks for any help on what may have happened and how to proceed processing the mud!!!

 

[Yggdrasil]

Can anyone recognize what I’ve done here? And hopefully how to fix it.

This is my process w/ the things I believe I messed up in bold.

- Mixed 500ml nitric with 500ml water (Should have added nitric over time)
- Used a torch to heat up scrap and added it to the acid.
-I was outside in the sun.
-The hot silver reacted quickly
-One spoon had a stronger reaction than the others so I didn’t add its handle. The handle says ss but does not test for silver.
I then put the beaker on the hot plate. (High)
- The acid boiled down to 600ml so I added 400ml more water.
- Boiled until an added sterling spoon no longer reacted.
- As it cooled the purple/grey mud settled under a clear blue liquid.
-the mud cannot be filtered
-I added distilled water and let the mud settle so I could get all the blue liquid I could.

I used an oxy torch and melted some of the mud along with baking soda. I was able to cast a small bead of metal that is very brittle, not magnetic and below 80% silver. The bead reacts with nitric.

I diluted some mud with water and added some hcl. A white precipitate formed. I’m guessing this is some silver from the solution that is the liquid component making the mud.

So… that’s my mess. Thanks for any help on what may have happened and how to proceed processing the mud!!!

SS means stainless steel so that is not Silver, most SS do not react much if at all in Nitric though.
If one spoon reacts more it probably is not Silver at all.

The mud can be anything that do not dissolve well in Nitric, so for the most part anything but Silver and Copper.
Tin paste for instance.

You need to sort your stuff properly.

No need to boil just keep hot at 70-90C.

Blue colour is Copper and white precipitate from salt/HCl is Silver Chloride which turn grey/purple in sunlight.

 

[PPDB]

Thank you for your reply.

I still have part of the spoon handle. It is mailable and reacts to nitric so I am confident it is not stainless.

I did spend quite a bit of time separating my sterling. I have points of it here. If I have a set of spoons for example I typically tested only one of the set. I had another spoon that looked to be the same as this one that tested as silver. They were obviously not the same and I should have noticed. But… I didn’t.
My plan now is to wash the mud the best I can and siphon off the silver nitrate. I’ll save the mud and processes it at a later time when I better understand what it is.

 

[PPDB]

It took me a while but I pressed through and got the mud filtered down to 35ml of the consistency of clay. I have a lot of dilute nitrate solution but I should be able to process it now. Then I’ll calculate my yield and will report back in case anyone is interested. Anyway.,,,

 

[BGDOCK]

I would like to take a try at this one . I had a batch of stock pot waste similar. It was cemented silver and silver chloride I put it in diluted sulfuric acid and a cast iron pan with nails that worked well . (Check out other methods in the silver section of Hookes book. )
Add dilute sulfuric acid to that decanted solids .
Work in small batches
Put in cast iron pan I used a old Allen wrench to stir
After it turns black put in a beaker / container
Do next batch
Cover with distilled water , rinse let settle rinse again
Dirty copper sulfur acid waste is iron sulfite
After rising I used a HCl boil and then rinsed again , rinse this well.

Jeff

 

[PPDB]

Ok. I will try this. Just cement out using iron? Copper won’t cement because of the sulfur?

 

[BGDOCK]

Copper cemented ( stayed on / adhered to ) on some the nails . But I considered that a bonus when cementing out .
Use a little heat or do it on a hot day
The silver will be a little dirty at first but two things
1.) It converted the silver chloride and cemented silver that had becomes mixed up in my stock pot waste.
2.) it’s pretty quick and just rinse well do a HCl hot treatment to get rid of iron and copper
Treat the waste solution from this w/ iron

 

[PPDB]

I ran a sample through your procedure. However, I was kind of sloppy with the process so I’ll try again tomorrow.

I didn’t boil in hcl, just hot water and hcl rinse. So I’ll do better.

The result of my sloppy process gave me two noticeably different sediments. One grey/tan and clouded the rinse. The other heavier, clumpier, and darker.

I have not yet processed the gray but was able to melt down the black. It was difficult to melt with my propane torch but was able to put a pea sized bead.

It does not test as silver using the test solution I have. My solution doesn’t test well under %90 though. It has a similar color to nickel. However, it has no magnetic response using four computer hard drive magnets. I would think that nickel would. So I’m not sure what it is.

I’ll do better tomorrow and also see if I’m able to collect the gray precipitate as well.

Dave, thank you for your input!

 

[BGDOCK]

Is that filtered mixture dry .
If it still damp cover with very hot water
If it stays in solution silver chloride
If it dissolves lead
I forgot the tin test ( hit the book)
Take a small sample and add a little lye to it see if it turns black thats another way to see if it’ contains silver chloride
I will try and post pics and more details in another thread

 

[BGDOCK]

Need to correct a mistake silver Chloride will settle out of solution not stay
Lead Chloride would stay in solution
I’m done rough day

 

[Yggdrasil]

Ok. I will try this. Just cement out using iron? Copper won’t cement because of the sulfur?

If you have precious metals in solution it will cement in Copper.
Iron will take the Copper and other elements too.

 

[Yggdrasil]

Copper cemented ( stayed on / adhered to ) on some the nails . But I considered that a bonus when cementing out .
Use a little heat or do it on a hot day
The silver will be a little dirty at first but two things
1.) It converted the silver chloride and cemented silver that had becomes mixed up in my stock pot waste.
2.) it’s pretty quick and just rinse well do a HCl hot treatment to get rid of iron and copper
Treat the waste solution from this w/ iron

If you get Copper on your Iron it means your Chloride was not washed enough.
The Chloride need to be clean.

 

[PPDB]

I’ve processed the nitrate solution and calculated 89% yield of the original sterling weight. I am happy with that considering… though there were a couple pieces of fine silver cast droppings included in that batch.

I dropped the metal from the purple mud sample using iron as suggested. This left a fluffy tan soot in the solution. The filtered soot burned away with the torch.

I don’t have the chemicals needed to make it easy, so I also followed the book on another sample to determine what metal I am left with. I think these processes require a little more experience to follow the subtleties in observation. I did my best.

I don’t think it is lead or tin. It has a high melting point and looks like nickel but has no magnetic response at all. I may have an alloy of sorts but then again, I would expect that to lower the melting point some.

I’m going to keep the rest of the mud in a jar for now and move on

 

[BGDOCK]

Can you put a cd rom magnet on a copper wire and see if you pull iron out of that waste mixture ?

 

[Yggdrasil]

I’ve processed the nitrate solution and calculated 89% yield of the original sterling weight. I am happy with that considering… though there were a couple pieces of fine silver cast droppings included in that batch.

I dropped the metal from the purple mud sample using iron as suggested. This left a fluffy tan soot in the solution. The filtered soot burned away with the torch.

I don’t have the chemicals needed to make it easy, so I also followed the book on another sample to determine what metal I am left with. I think these processes require a little more experience to follow the subtleties in observation. I did my best.

I don’t think it is lead or tin. It has a high melting point and looks like nickel but has no magnetic response at all. I may have an alloy of sorts but then again, I would expect that to lower the melting point some.

I’m going to keep the rest of the mud in a jar for now and move on

What do you mean by this?

I dropped the metal from the purple mud sample using iron as suggested. This left a fluffy tan soot in the solution. The filtered soot burned away with the torch.

Dis you cement on Iron?

 

[PPDB]

I used nails mixed in a cast iron mold as suggested.

 

[Yggdrasil]

I used nails mixed in a cast iron mold as suggested.

Ok, then all what is left would be waste Ferrous Sulfate if the AgCl was properly cleaned.
My confusion came from that you used the term dropped which is normally used when dropping a solid from a liquid.

 

[Martijn]

Can anyone recognize what I’ve done here? And hopefully how to fix it.

This is my process w/ the things I believe I messed up in bold.

- Mixed 500ml nitric with 500ml water (Should have added nitric over time)
- Used a torch to heat up scrap and added it to the acid.
-I was outside in the sun.
-The hot silver reacted quickly
-One spoon had a stronger reaction than the others so I didn’t add its handle. The handle says ss but does not test for silver.
I then put the beaker on the hot plate. (High)
- The acid boiled down to 600ml so I added 400ml more water.
- Boiled until an added sterling spoon no longer reacted.
- As it cooled the purple/grey mud settled under a clear blue liquid.
-the mud cannot be filtered
-I added distilled water and let the mud settle so I could get all the blue liquid I could.

I used an oxy torch and melted some of the mud along with baking soda. I was able to cast a small bead of metal that is very brittle, not magnetic and below 80% silver. The bead reacts with nitric.

I diluted some mud with water and added some hcl. A white precipitate formed. I’m guessing this is some silver from the solution that is the liquid component making the mud.

So… that’s my mess. Thanks for any help on what may have happened and how to proceed processing the mud!!!

How did that spill on the second picture happen and how did you clean it and dispose of it? Does anyone else walk that workshop? wife kids, Pets?
Are you changing shoes going in and out?
Are you working in a tool shop? Your iron and steel tools quickly corrode from HCl fumes.

That green stain on the floor is a toxic mess and a hazardous contamination that could end up anywhere, in the neighbors kids organs, e.g.

So are you in a position where we should give you advice on how to resolve your challenge, or do we need to get you up to speed on safety practices first?
If you consider this picture GRF-worthy, I seriously wonder about your awareness of the risks involved with this hobby.

Martijn.

 

[billgold]

Some clarification please.

Is that first picture the silver recovered out of the nitrate solution?

Is that 89% recovery - 89% of the calculated original silver content or 89% of the original sterling silver weight?

 

[Wonka]

Can anyone recognize what I’ve done here? And hopefully how to fix it.

This is my process w/ the things I believe I messed up in bold.

- Mixed 500ml nitric with 500ml water (Should have added nitric over time)
- Used a torch to heat up scrap and added it to the acid.
-I was outside in the sun.
-The hot silver reacted quickly
-One spoon had a stronger reaction than the others so I didn’t add its handle. The handle says ss but does not test for silver.
I then put the beaker on the hot plate. (High)
- The acid boiled down to 600ml so I added 400ml more water.
- Boiled until an added sterling spoon no longer reacted.
- As it cooled the purple/grey mud settled under a clear blue liquid.
-the mud cannot be filtered
-I added distilled water and let the mud settle so I could get all the blue liquid I could.

I used an oxy torch and melted some of the mud along with baking soda. I was able to cast a small bead of metal that is very brittle, not magnetic and below 80% silver. The bead reacts with nitric.

I diluted some mud with water and added some hcl. A white precipitate formed. I’m guessing this is some silver from the solution that is the liquid component making the mud.

So… that’s my mess. Thanks for any help on what may have happened and how to proceed processing the mud!!!

There iron and copper in it. I get the same thing often.