First attempt at silver refining

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After drying it sat in my toaster over for couple of hours heres the weight dry.

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For batch 3
Its hard to make out but its 624.9, the weight of the empty vessal weighs in at 306.59 grams leaving me with 318.31 grams yeild. I started with 347.11 of clean sterling. Giving me a recovery of 91.7 %. Not to bad

For batch 4 i can not calulate a yeild due to the fact that two of the spoons where brass. I poured a little bar with the cement i got from this batch pictured below.

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I took this small bar and the 10 oz bar i poured above to my LCS who has an XRF.

He tested the 10 oz bar and it came in at 99.92 AG 0.08 CU
The little bar that came from the dirty batch came in at 98.6 AG and 1.4 CU.

Not bad either all things considered.

Also stopped at one of my favorite thrift stores and picked up my first piece of corningware, this should make my life easier.

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Well the time has come, i have gotten enough cement silver to explore the electrolytic silver cell, so i have the parts coming and will begin construction this weekend.

Cheers
 
on to batch 5 , i stepped up the quantity this time to 500 grams of some ugly sterling bars i poured when i was learning to melt.

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As per the steps, i melted this into shot and added a little bit of undigested shot from batch 4.

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With the advice i have recieved this is the cement setup now, the stainless steel welding rod and some of my copper pours with some copper ground wire. I used new wire everytime i add it but the bar i grind the oxidation layer off.

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and this is my filtered solution.

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now i did not plan, nor was i expecting to digest all of the shot i poured but i added it anyway as i know its better to be left over with some undigested silver rather than free nitric in the solution. Its worth noting that 350ml of 70 percent nitric consumed quite a bit more sterling than i expected.

I started with 521.41 grams of shot, and i was left with 66.21 after i exhausted all the nitric in the reaction.

Basically 350ml 70% / 350ml distilled water ate 455.2 grams of sterling, or my 70% nitric is actually stronger.

The reaction vessel is covered and being heated of course.

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As expected, since i consumed all the excess nitric in the reaction when i put in the copper for cementation nothing happened after a few minutes. So i added 2 ml of nitric and it took off. I had to step away for an hour but when i came back, something very interesting happened. I had beautiful crystals growing and a blue stripe within the solution from where all the silver was removed. Of course i stirred it and redistributed everything but it was indeed interesting. The pics where cool too.

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You said this.
I started with 521.41 grams of shot, and i was left with 66.21 after i exhausted all the nitric in the reaction.

Basically 350ml 70% / 350ml distilled water ate 455.2 grams of sterling, or my 70% nitric is actually stronger.
Here how I would have did it. I had 350 grams of Sterling 350ml of distilled water and 420ml of 70% Nitric Acid.

Here is a link how to do it.

https://goldrefiningforum.com/phpBB3/download/file.php?id=44986
 
jmdlcar said:
You said this.
I started with 521.41 grams of shot, and i was left with 66.21 after i exhausted all the nitric in the reaction.

Basically 350ml 70% / 350ml distilled water ate 455.2 grams of sterling, or my 70% nitric is actually stronger.
Here how I would have did it. I had 350 grams of Sterling 350ml of distilled water and 420ml of 70% Nitric Acid.

Here is a link how to do it.

https://goldrefiningforum.com/phpBB3/download/file.php?id=44986

Per the underlined -----------

There is no such thing as --- IT TAKES - or - YOU NEED --- x% (say 68 - 70 %) nitric to dissolve x amount (say 1 gram) of silver (or copper)

In other words - there is "no such thing" as an exact calculation of how much acid you need to dissolve an exact amount of metal

That is because how much acid to how much metal depends a great deal on the conditions involved in the dissolving of the metal --- in other words - depending on the conditions - it "may" take more acid - or - less acid to dissolve the amount of metal you are dissolving

I have posted about this a number of times in the past - here is a link to one such thread (which has a link to another one of my post on this subject)

:arrow: Dissolving the Copper in Sterling (nitric Qty?)

This is especially import to understand when making your electrolyte for your silver cell because you don't want to end up with "a lot" of free nitric in your electrolyte --- & for that matter you don't want to be wasting nitric because you are using "poor conditions" to dissolve your silver

Kurt
 
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Kurt,

When we'd make up our electrolyte we'd always leave extra silver in the bottom in bar form. We'd start with a known quantity of dry cement, dissolve it, leave a bar in there to kill off excess nitric and then weigh the solution and titrate a 5.000 g sample of it in duplicate.


GSracer, you might consider skipping the Cu reduction and going with the addition of HCl. If it were me, I'd pull a small sample of the pregnant (as in it's full of silver), filtered Ag solution and then I can test how much HCl it takes to precipitate 95% of the Ag. I don't even need to standardize the HCl. I would just take my concentrated stuff, dilute it down 10X and see how many drops it takes to precipitate a known mass or volume of that solution.

I don't want to precipitate all of the Ag, just most of it:

AgNO3 + HCl = AgCl (precipitate) + HNO3

If I do not add overmuch HCl, I can reuse the nitric acid for dissolving more sterling and lower my unit cost per ounce. Also, adding an air bubbler to the reaction helps produce nitric acid in situ by the following reaction.

O2 + 4 NO2 + 2 H2O = 4 HNO3
Once upon a time, a large company doing 40 tons of Ag per week in nitric was using a pressurized version of that reaction.

If you then take the AgCl, you can cement it with much cheaper iron and sulfuric and some tumbling. This might not produce less liquid, but it certainly costs less in both nitric and copper and the silver metal obtained can be very high quality if washed with the right flux mixture!
 
jmdlcar said:
I am STOP saying or writing anything to anyone that write a message.
No need for that sir. Sharing is caring and you have the best intentions to help and contribute. That's exactly what this forum is about.
We correct (sm)all details so others that read this will not be misinformed.
We never stop learning. None of us. Love this forum.

I have limited knowledge in this field being a hobbyist and have been learning by reading a lot and the corrections i got from members.

Since these gentlemen gave me so much for free i want to give some back whenever i can about things i feel confident enough about to advise new members.
Next level things i leave alone for the jedi's. And they have said all of that basic stuff more than enough.
Only when someone is lost or asks basic things I respond if no one else has.
And i have been put in my place more than once. And i thank them for it. As long as it's polite and constructive.
Martijn.
 
Lou said:
Kurt,

When we'd make up our electrolyte we'd always leave extra silver in the bottom in bar form. We'd start with a known quantity of dry cement, dissolve it, leave a bar in there to kill off excess nitric and then weigh the solution and titrate a 5.000 g sample of it in duplicate.

Lou

Not sure what your point is - but yes you can certainly make your electrolyte with cemented silver as the cement silver should be relatively low in copper (if done right) it is just my preference to use some of the crystals from my cell for my electrolyte - & yes you want to make sure there is some silver remaining when the reaction is "done" to insure there is no free nitric

For what its worth - there are (only) a couple reasons why I even run my "small" silver cell

1) I have a silver buyer that pays me 5% over spot for my silver cell refined silver - he is a Hmong silver smith that makes ceremonial Hmong jewelry - the "true" Hmong traditional/ceremonial jewelry is made of 999 (plus) silver (not sterling) so he likes my silver cell silver

2) I always end up getting a few large crystals when I run my cell - the crystals that run from 2.5 grams to 7 grams are picked out & sold as crystals because I am able to get 5 to 10 times spot for them depending on their size, shape &/or crystal structure

Other then that - sterling goes direct to a refinery as I get paid the same or 925 as I get paid for 999 so it doesn't make a lot of sense to spend the time & chem cost to refine it myself

lower grade &/or un-known silver (such as contact points or silver recovered from gold filled etc.) gets dissolved & cemented - poured to kilo bars - XRF'ed - & other then "some" of it run in my cell - it goes to the refiner for the same reason sterling goes to the refiner

Kurt
 
JMD,

The point i was making (especially after reading numerous threads on the subject) is there is no set amount of nitric for dissolving silver. Especially if you are applying heat and have the reaction vessel covered. I have found on the 5 batches i have ran that it takes considerably less nitric to digest the silver.

What i typically do is weigh the amount of metal i want to process, for the sake of numbers lets say 250 grams of sterling. I add 250ml of water, then 100 ml of nitric, cover, heat and see how the reaction goes. I typically add 50 ml at time watching the fume production towards the end i add 10 ml increments until i have just a little un reacted metal left on the bottom. This ensures no free nitric in the solution which will cause problems during cementation. Had i added the prescribed amount of nitric in the beginning. Each batch would have had a severe excess of nitric in solution. Just something to note when you start yourself. :)


Kurt,

As to make your point, i dissolved 180 grams of silver cement mixed with 120 grams of 999 bullion coins in just 200 ml of nitric for my electrolyte.

Lou,

Im going to attempt to learn the silver chloride method when i process my waste bucket. That will be a learning curve for sure. But thanks for the info!


So to update, i have on hands 1680 grams of cement powder, and my supplies came in so time to build my silver cell.

I ordered the adjustable power supply and the stainless bowl, however i wanted to try something different. I had some 316 stainless plate from a previous project in the garage so i cut a piece to fit inside a 2000ml beaker, and tigged a 3/16 rod to the plate. I inuslated the rod with 2 layers of polyolefin heat shrink.

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I used 120 grams of 999 silver bullion and 180 grams of my lightest cement powder to make the electrolyte. Giving me 150 g/l.

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I poured a few small bars to use in my anode basket, the basket is made of 2 layers of walmart muslin cloth.

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now before you say it, i know the cathode anode distance is further than the prescribed 4.5 inches. However i didnt realized that till moments before i hit "ON" at the power supply. However it was late so i figured what the hell. Im going to make a new cathode today to shorten the distance. I will also be pouring more cement shot to fill the basket as i also ran out of propane last night. The basket can easily fit 10 oz bars.

The cathode surface area is roughly 10.4 sq inches, and i was able to put 3.0 volts and 2.29 amps.

Here is a shot of the basket. Im already seeing black residue and decomposition in the anode basket.

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This is the growth within a few minutes after turning the cell on

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And here is after running for exactly 12 hours.
 

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jmdlcar said:
I am STOP saying or writing anything to anyone that write a message.

jmdlcar

I did not mean to offend you & am MOST CERTAINLY sorry if I did :!:

Not sure where to even start here - but will try

You have been a member for about 10 years now - but based on your recent questions you are just beginning your first attempts in silver refining (so it's a learning process)

In one of your threads you asked the question - "how much nitric do I need to dissolve X amount of silver" ?

In reply to that Ralph (palladium) posted the link to the PDF acid work sheet - & there is nothing wrong with that PDF

Ralph is one of our "most respected" members (& a member I VERY MUCH respect) and those numbers posted in that PDF are true - BUT - they are only true "To a Point" --- in other words generally speaking those numbers are true - but they are not absolutely true --- that is because although generally speaking those numbers are true - the amount of actual amount of acid it will take to dissolve a given amount of metal can & WILL change based on the conditions under which the metal is being dissolved --- THAT is true whether you are dissolving gold, silver, copper or other (normally base) metals

In other words - those (PDF) numbers are a general "rule of thumb" but NOT an "absolute law"

Therefore - IF (the big IF) you follow those numbers as a absolute law - you will more often then not - find yourself wasting acid

That is because using those numbers "to the letter of the law" - you will find - that depending on the conditions used in dissolve a given batch of metal - more often then not - one of two things will more likely (then not) happen

1) all your metal will NOT dissolve - so you will need to add more acid - which in turn means you are wasting acid

2) all your metal will dissolve BUT there will still be "free" acid left (so unless you have more metal to add - to use up that free acid) again you are wasting acid

Point # 2 (above) is one of the most common mistakes that new members run into when they dissolve gold with AR --- & then when they use to much nitric in their AR they can't get their gold back (the gold wont drop back out of the AR) so we end up telling them that "their problem" is to much free nitric in the AR so they need to de-NOx the AR to remove the free nitric before their gold will drop

The reason that they end up with free nitric in their AR is because before coming here to the forum - they find info elsewhere on the internet with a "general rule of thumb" for dissolving gold

The general rule of thumb - for dissolving gold - is to use 1 ml 70% nitric with 3 ml HCl to dissolve 1 gram of gold - and that "MAY'" be close to true if you are trying to dissolve a solid gold coin

However - more often then not - they are dissolving gold foils recovered from a batch fingers - & that changes the condition of dissolving the gold --- in other words - there is a difference between dissolving a one ozt gold coin & dissolving one ozt of gold foils

That difference (which is a condition) is surface area --- an ozt of gold foils has MUCH more surface area then a solid gold coin

Therefore - because the gold foils are VERY thin with LOTS of surface area - the acid does not need to work anywhere near as hard to dissolve the gold - which in turn means it WONT take as much acid to dissolve the gold - compared to dissolving a sold gold coin - which in turn means if you use the "rule of thumb" (1/3 nitric/HCL to dissolve a gram gold) to dissolve gold foils - you ARE going to end up with with free nitric in your AR - which then means you have to de-NOx the AR to get rid of the free nitric - or your gold will not drop - which in turn means you wasted acid in the first place

The same holds true whether you are dissolving gold, silver, copper or some other metal

How much acid it takes to dissolve a given amount of metal WILL change depending on the conditions under which you are dissolving the metal --- in other words - depending on conditions - it may take more acid - or it may take less acid - then the (so called) rule of thumb numbers

the bottom line is that if you follow the rule of thumb numbers - as an absolute law (as in IT TAKES) you will in fact find yourself wasting acid

Therefore - once you understand how conditions effect the amount of acid you need to dissolve a given amount of metal - you can use those conditions to your advantage - so you need to understand the conditions that effect the actual amount of acid it will take to dissolve a batch of metal (& there is NO absolute here - it is "a bit" of a guessing game with each batch)

1) surface area - it takes more acid to dissolve (say) a solid kilo bar of silver then it take if you dissolve (say) that same kilo of silver melted & pour to silver shot --- that's because by pouring the silver to shot you create a whole "lot" more surface area - so the acid does not have to work as hard at dissolving the silver - so you will use less acid

2) dissolving the metal in a closed vessel compared to dissolving the metal in an open vessel - if you dissolve the metal in an open vessel (no cover on the beaker/bucket or pot) it will take more acid then if you put a cover on the vessel - that's because by keeping the NOx in the beaker (or vessel) helps get more use of the acid as "some" of that NOx gets re-absorbed back into the solution during the reaction - instead of letting all the NOx go out the top of the beaker

3) when dissolving silver (or copper) - if you use about half again the (so called) recommended amount of water (distilled) you will get better use of the acid - that's because the NOx stays in the solution better (in stead of just gassing off) thereby you will get more full use of the acid during the reaction

4) Heat makes a difference - to little (or no) heat makes the acid work harder (not the same as - but kind of like surface area effects acid consumption) & on the other hand to much heat will cause NOx to be driven out of the solution during the reaction --- therefore you can start out with your batch on the hot plate to get the reaction started - once it is getting going but not full blown - turn the heat off & the heat of the reaction will do its own thing - then when the reaction is slowing down - turn the heat back on until you are done with the batch --- this will give you better use of your acid

Taking into consideration & using these conditions - I have dissolved successfully (although only a couple times) as much as 500 grams silver with only 350 ml 68% nitric (so .7 ml acid per gram silver - that's 5 tenths of a ml less acid then the "recommended" 1.2 ml acid per gram)

On the average (so sometimes more & sometimes less) - using those conditions to my advantage - I would be willing to say I get away with using only about .9 ml of 68% nitric per gram of silver when doing a batch of silver

To put that in perspective - when I make my electrolyte for my silver cell - I do it in 500 gram (silver) batches - on the "average" I am able to dissolve that 500 grams with "about" 450 ml 68% nitric --- so on a 500 gram batch I am saving "about" 150 ml of nitric --- in other words - according to the rule of thumb - in theory - it should take 600 ml acid to dissolve 500 grams silver - but on average I get away with only "about" 450 ml acid

My point in all of this is that the PDF Ralph posted is actually only a rule of thumb (not an absolute law) - therefore - as a rule of thumb - depending on conditions - it may take more acid - or less acid then the rule to dissolve a given amount of metal --- & IF you use those conditions to your advantage you can almost always (if not always) get away with less acid

Kurt
 
First off I know I been here 10 years now and I started with Gold because it didn't take much to get $$$ but some one wanted more them me and they took it. It was 10grams I did. So I just quit doing it.

Now what happen now I wanted to start over but this time I went with Sterling Silver that's why I ask this question "how much nitric do I need to dissolve X amount of silver" to get a idea so I would get a idea.

So I quest when I do my first batch and have 200 grams of Sterling I would use 200 ml of Distilled water and start with 50ml of 70% Nitric Acid then add 50ml tell I get to 100ml and then I go to 10ml if then I have a little Sterling left I will stop. I wanted to do it right so I wouldn't have any waste.

I have my equipment when I did Gold but I did buy a Stainless Steel 304 2 quart stock pot to process the Sterling Silver and copper to cement the Silver. I know 2qt stock pot is no big but I won't process more then 200 grams at a time Nitric Acid.

Then I will do a Silver Cell it get 999 I hope.
 
jmdlcar said:
First off I know I been here 10 years now and I started with Gold because it didn't take much to get $$$ but some one wanted more them me and they took it. It was 10grams I did. So I just quit doing it.

Now what happen now I wanted to start over but this time I went with Sterling Silver that's why I ask this question "how much nitric do I need to dissolve X amount of silver" to get a idea so I would get a idea.

So I quest when I do my first batch and have 200 grams of Sterling I would use 200 ml of Distilled water and start with 50ml of 70% Nitric Acid then add 50ml tell I get to 100ml and then I go to 10ml if then I have a little Sterling left I will stop. I wanted to do it right so I wouldn't have any waste.

I have my equipment when I did Gold but I did buy a Stainless Steel 304 2 quart stock pot to process the Sterling Silver and copper to cement the Silver. I know 2qt stock pot is no big but I won't process more then 200 grams at a time Nitric Acid.

Then I will do a Silver Cell it get 999 I hope.



That's exactly what i would do. Just watch the fume production.


kurtak said:
Gsracer

Read what I posted concerning anode bags in this thread as well as Lou's comment to what I posted

:arrow: Copper cell

also for a small cell read this

:arrow: Can only get coral like silver crystals

Kurt


Kurt i did read both of those threads.

This is the cloth i purchased

https://www.walmart.com/ip/Waverly-...-Precut-Natural-Muslin-Fabric-1-Each/49332641
But i think i got the wrong one, see below.

Well this morning this is what it looked like.

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I started making my different cathode for my beaker, i went with a slighlty different design. Half circle and lighter weight so i can suspend it closer to the anode basket. And it would have space so when i would knock down the crystals they would fall to the bottom and hopefully allow me to run the cell for longer period of time. It is not at 4.5 inches below the anode basket. It gives me a surface area of 7.92 inches.

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So i began dissembling the cell to harvest and change out the cathode. This is what my anodes looked like when i removed them.

And the sludge in the basket.

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However when i removed the basket i placed on another beaker, i noticed the sludge was dripping through into the basket. The cell itself was completly clean with no residue this only happened when i moved the basket. Is it possible the cloth i have is the incorrect one or my basket has to many / to large of holes?

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In either case , i filtered my electroylite and placed a new doubled muslin cloth filter in there and started it back up.
 
With in minutes of starting.

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After running for just over two hours.


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This is the dried silver cell from running for 14 hours. 141.1 grams or 4.56 troy oz not incuding the beaker.

It sure is pretty. the picture does not do it justice really, although im worried it could be contaminated from the issue i posted above.

Critiques , thoughts welcome

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For me the second one look a lot clear and a lot better to. That another item I need to buy to filter Silver.
 
Can someone tell me what cause the sludge in this picture?
https://goldrefiningforum.com/phpBB3/download/file.php?id=45435&t=1
 
Just to update, this cathode seems to be running more efficiently.

With the previous cathode thickness and spacing i could get 3.49 volts @ 2.49 amps.

With this new thinner and closer cathode im running at 3.49 volts @ 2.56 amps.

So i figured i was going to need more silver to run through. I melted 15.26 troy ounce to run. Instead of bars i decided to use shot this time.

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Interesting comparison from left to right

sterling shot for digestion, cement silver shot, silver crystal from the cell.

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about 20 ounces in the basket, once i poured the shot something interesting happened. The amps went from 2.56 amps to 3.38 amps at 3.49 volts.

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growth at hour 5

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