How Far to Refine Your Silver?
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It seems to be difficult to get all the silver chloride out of the silver (or at least time consuming). I don't want to put silver back in the blender for fear of making all the silver fine as powder and difficult to clean. I'm thinking of going to Plan B, which is to buy some nitric acid. Here's my idea:
I had 800 g AgCl, which is now maybe 90% silver and 10% AgCl all mixed up, with some tiny chunks of AgCl coated with silver. My thought was to dissolve the silver with nitric acid (should take less than 1 liter, right?) and what doesn't dissolve should be AgCl only. I can then reprocess the AgCl, redissolve with nitric and repeat until the AgCl is all gone. I would then take the silver nitrate and drop the silver with copper, or maybe electrolyze until depleted, and then drop the remainder with copper.
Will this work? Also, since I started with AgCl and not sterling, I don't expect much copper. Will dropping with copper contaminate the silver? Does it really matter if I will be paid by the purity after analysis anyway?
Thanks.
I had 800 g AgCl, which is now maybe 90% silver and 10% AgCl all mixed up, with some tiny chunks of AgCl coated with silver. My thought was to dissolve the silver with nitric acid (should take less than 1 liter, right?) and what doesn't dissolve should be AgCl only. I can then reprocess the AgCl, redissolve with nitric and repeat until the AgCl is all gone. I would then take the silver nitrate and drop the silver with copper, or maybe electrolyze until depleted, and then drop the remainder with copper.
Will this work? Also, since I started with AgCl and not sterling, I don't expect much copper. Will dropping with copper contaminate the silver? Does it really matter if I will be paid by the purity after analysis anyway?
Thanks.
I do not see why it would not work.
If you can afford the nitric.
If you can afford the nitric.
A
Anonymous
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I agree with butcher. If you can afford it, use the nitric. It'll dissolve the silver and it'll be easier for you to recover it later on, especially if copper is the main/only contaminant.
Kevin
Kevin
OK, I finally acquired some nitric acid locally. It's 50% nitric, but it is 50% v/v. I've searched the forum but I can't find anything on what the recommended 70% nitric actually is. Are we talking w/v or v/v or what? Everybody always just says use something like 1.2 ml 70% nitric to dissolve 1 g of silver. I need to know as I want to be sure I am dissolving enough silver for the amount of 50% v/v nitric that I'm using. I only have 1 liter and something like 600 g of silver. Anybody know the conversion from 50% v/v to 70% of whatever it is?
A
Anonymous
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Why not take 1 gram of silver and 1.17ml of Nitric and 1.17ml of water or peroxide and see how fast it'll dissolve. I'm using 70% nitric (actually it's 69.5%) and it starts to dissolve silver within seconds after putting them in the acid.Bushka said:
If anything, I would suspect the nitric would take a bit longer to dissolve the silver. Then again, it may be just as 70% if you were to use a little heat to the vessel.
w/v and v/v.... What are you talking about? weight per volume and volume per volume?
Kevin
commercial azeotropic nitric acid 68% w/w
http://www.thechemicalblog.co.uk/what-do-vv-ww-wv-andvw-mean/
http://www.thechemicalblog.co.uk/what-do-vv-ww-wv-andvw-mean/
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Anonymous
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Thanks butcher, now I understand and I'll be able to relate to it when I see it again in threads.butcher said:
Kevin
So I take it then that when everybody says 70% nitric they are talking 68% w/w. I don't suppose anybody has already done the math to convert that to v/v??? I tried to dissolve a little silver last night, but it was bitterly cold and my heating set up was less than well thought out. I was hoping the reaction would get going quickly enough sitting in some warm water. Between that and a hair dryer I did get a little reaction but it never took off. Then when I checked on things later the warm water bath had frozen solid! I'll try plan B tonight.
A
Anonymous
Guest
Not really, when some people say 70% nitric, they're talking about 70% nitric. Because, from what I have learned so far, 68%+ is also considered 70%, or, at least it's just as reactive as 70%. So, if you have 68% nitric, it should dissolve your silver, if it is indeed silver.Bushka said:
I hav no idea, but if it were me, I would first measure my water I'm going to add, then measure the nitric, then add the nitric to the water. Once your silver is in the solution, wait a few seconds and a reaction should start. If a reaction doesn't start, add more nitric, (about 3 ml at a time) wait for the reaction after each addition of nitric. If still no reaction, then add some heat to the vessel. If still no reaction, then either your Nitric is spent/too weak or the metal you're trying to dissolve isn't silver, or it's a metal nitric won't dissolve. I can't see it not dissolving your material, if it is indeed silver.Bushka said:
You should have added a bit more nitric to the solution. I'm almost sure, but not positive, but if it's that cold outside, then a hair dryer probably wouldn't be sufficient enough to heat the vessel. How was the dryer positioned? To the side of the vessel? Real close to the side of the vessel? Blowing from the top of the vessel? How cold was it outside?Bushka said:
I'm nowhere near a professional in refining silver, but I've refined silver (.925) and I've had great success so far and not a single problem as of yet.
As far as what you should yield from what you have is just a maybe, possibility or hopefully. If haven't processed that same exact bath of material or even closely similar to it, you can't tell what you should get. I can see you saying "I hope I get X amount of grams out of this".
You never showed any photos of the material you was working with. Do yourself a favor and take pictures along with notes. It can help others determine what is going on and what must have went wrong during the process(es). I do that myself, which I've did, and when I uploaded images of what was what, the members here were able to give a general idea of what may have happened, just by looking at the pictures. Believe me... take pictures and take notes. It'll make the world of difference when you ask for help.
But get you a hot plate and a heat gun. A hair dryer is good for certain things, (I even have one myself), but for the refining and processing of gold and silver, I'll use a heat gun, if needed and not a hair dryer.
Kevin
Thanks Kevin. I actually did post a number of photos earlier in this thread, which has been mostly about trying to convert AgCl to silver through lye and syrup. As you may recall from above, I've decided to bite the bullet and get the nitric. I'm just being super cautious with the first test of dissolving my cement. I'm looking for a cheap (free?) hot plate but I'm concerned even with that because I'm using an old Skippy jar, which isn't pyrex. I don't want to over heat the bottom and end up with cracked glass and silver nitrate everywhere. I was able to heat my first test batch (50 ml nitric, 50 ml dist. water) in a dehydrator, which is a metal box that blows hot air. I don't want to use this again as it's really meant for food, but I really didn't want partially reacted nitric/silver sitting around the house. It looks like heating it up helped the reaction a lot, as did adding much more silver cement. It never got to the point where it was bubbling and frothing like you see on Youtube, but I think you probably lose more NO2 that way, too. I kept a plate of glass over the jar during the reaction. I kept adding silver to excess, and I think now most of what is sitting on the bottom is more pure silver chloride. I'll separate that out and give it the lye treatment again. So if I have enough nitric, I'll process all my cement, which could well be 10 or 20% AgCl. Then I'll lye/karo the AgCl and redissolve with nitric again... repeating until all AgCl is gone.
Do you use plain glass jars or pyrex lab glassware, and do you heat on a hot plate?
Do you use plain glass jars or pyrex lab glassware, and do you heat on a hot plate?
A
Anonymous
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No# 1. STOP using that Skippy jar with heat. You're asking for trouble.Bushka said:
No# 2. Go to the thrift store/goodwill and buy you a hotplate and some glass jars. I have plenty that are my beakers and they're thicker and taller than beakers too. Not sure if they're heat tested, but I use them as vessels. I do have and use Pyrex, but talk is not to use them and use Corning Ware.
Personally, I use Pyrex dishes to incinerate/heat on a hotplate and haven't had a problem as of yet. As far as incinerating, I've used a MAPP torch on my Pyrex numerous times and nothing went wrong (not saying it never will). But the trick to keep it from going into thermal shock (even in the summertime) is to place it on top of insulating blanket (the type used for insulating the inside of kilns and furnaces). The insulation (my theory) keeps the glass from coming into contact with the surface (wood/glass/metal/cement), which I believe causes them to crack/break/shatter, and helps to keep the glass hot, yet, cool enough to not overheat.
If you do use a Pyrex on a coil hot plate (I do it myself), just place it in a bigger pot or metal vessel, so that way, if it should crack, you won't lose anything. But, putting pyrex in a metal vessel and then placing it on a coil hot plate should pose no threat to the pyrex dish. Depending on what you're working with, you can even ad some water to the vessel, then place the pyrex inside.
No# 3. If that dehydrator has been used to do any processing, I hope you know it should NEVER EVER AGAIN be used for human consumption. If it works for you, you might as well keep using it because I hope you don't plan on dehydrating and more food with that. I'd hate to hear that you dehydrated foods, vacuum sealed them, then years later when you opened them up and ate them, you got poisoned. Trust me on this one. It can NEVER be used again for food consumption. Period.
I know there are more than one way to do a lot of what we do here, but, for me, I would simply dissolve my silver in Nitric/Peroxide, then add equal amounts of distilled water, add clean copper and let it drop the silver. Rinse with plenty of hot/boiling distilled water, let it dry, then melt the silver. Done deal.
To each their own, but using lye, syrup, salt, and other chemicals/powders to me, are just more steps to achieve the same exact thing. I'm not saying I'll never try them one day, but for now, why would I bother with all those steps? Dissolve. Drop. Wash/Rinse/Dry. Melt. To me, it's that simple, when it comes to silver.
Kevin
Hi Kevin. I had a couple of replies:
I poured a pot of boiling water in the Skippy jar I'm using just to see if it could take some heat, and it did not crack. So, I went ahead and used it for my first little test (sitting inside a wide glass bowl). I still don't like the idea of using it on a hot plate, though. When I mentioned Pyrex, I was thinking about the lab glassware that everyone uses, not stuff for kitchen use. I think those are fine on hot plates. Are the beakers you use from the thrift store very thick? I would think thick would be more likely to crack than thin, but I guess if it works it works.
I found 3 hot plates at the thrift store yesterday, and all three were barely warm to the touch. Maybe ebay is easier.
I'm amazed that you can actually melt silver in a pyrex bowl. I was just going to use a block of wood or something. I do have 2 small crucibles so maybe I'll use those, too. I was reading from someone in this forum that MAPP can overheat silver and vaporize some, and he recommended propane. Can't remember who recommended that. Have you tried to work with propane?
I think you are overreacting a little to the use of the dehydrator. This was a very mild paced reaction and for the most part I left the front door of the dehydrator off. Hot air was blowing from the back of the unit and out the front. I only use the dehydrator for making treats for our pets, not that that makes it less important. I've inspected the interior (stainless steel), wiping it with my finger and putting my nose to it. I let it run for an hour afterwards and will wipe it with a damp towel with bicarb tonight. In short, I think by putting a glass cover on the jar, much of the NO2 refluxed back down and/or went straight outside. I understand your concern, but if you saw what I'm talking about you might get my point. In any case using that was a one time thing just to get this batch reacted.
Also, I am planning to do what you say - drop with copper and be done with it. However, the bulk of this thread is talking about the trouble I'm having converting the AgCl to Ag. It's the AgCl, not the AgNO3 that I'm planning to reprocess with lye. I'm using the nitric to separate the silver (good) from the silver chloride (bad).
Now I gotta go find a cheap hot plate.
I poured a pot of boiling water in the Skippy jar I'm using just to see if it could take some heat, and it did not crack. So, I went ahead and used it for my first little test (sitting inside a wide glass bowl). I still don't like the idea of using it on a hot plate, though. When I mentioned Pyrex, I was thinking about the lab glassware that everyone uses, not stuff for kitchen use. I think those are fine on hot plates. Are the beakers you use from the thrift store very thick? I would think thick would be more likely to crack than thin, but I guess if it works it works.
I found 3 hot plates at the thrift store yesterday, and all three were barely warm to the touch. Maybe ebay is easier.
I'm amazed that you can actually melt silver in a pyrex bowl. I was just going to use a block of wood or something. I do have 2 small crucibles so maybe I'll use those, too. I was reading from someone in this forum that MAPP can overheat silver and vaporize some, and he recommended propane. Can't remember who recommended that. Have you tried to work with propane?
I think you are overreacting a little to the use of the dehydrator. This was a very mild paced reaction and for the most part I left the front door of the dehydrator off. Hot air was blowing from the back of the unit and out the front. I only use the dehydrator for making treats for our pets, not that that makes it less important. I've inspected the interior (stainless steel), wiping it with my finger and putting my nose to it. I let it run for an hour afterwards and will wipe it with a damp towel with bicarb tonight. In short, I think by putting a glass cover on the jar, much of the NO2 refluxed back down and/or went straight outside. I understand your concern, but if you saw what I'm talking about you might get my point. In any case using that was a one time thing just to get this batch reacted.
Also, I am planning to do what you say - drop with copper and be done with it. However, the bulk of this thread is talking about the trouble I'm having converting the AgCl to Ag. It's the AgCl, not the AgNO3 that I'm planning to reprocess with lye. I'm using the nitric to separate the silver (good) from the silver chloride (bad).
Now I gotta go find a cheap hot plate.
A
Anonymous
Guest
I do not melt silver in pyrex. I said I incinerate in a pyrex.Bushka said:Hi Kevin. I had a couple of replies:
I poured a pot of boiling water in the Skippy jar I'm using just to see if it could take some heat, and it did not crack. So, I went ahead and used it for my first little test (sitting inside a wide glass bowl). I still don't like the idea of using it on a hot plate, though. When I mentioned Pyrex, I was thinking about the lab glassware that everyone uses, not stuff for kitchen use. I think those are fine on hot plates. Are the beakers you use from the thrift store very thick? I would think thick would be more likely to crack than thin, but I guess if it works it works.
I found 3 hot plates at the thrift store yesterday, and all three were barely warm to the touch. Maybe ebay is easier.
I'm amazed that you can actually melt silver in a pyrex bowl. I was just going to use a block of wood or something. I do have 2 small crucibles so maybe I'll use those, too. I was reading from someone in this forum that MAPP can overheat silver and vaporize some, and he recommended propane. Can't remember who recommended that. Have you tried to work with propane?
I think you are overreacting a little to the use of the dehydrator. This was a very mild paced reaction and for the most part I left the front door of the dehydrator off. Hot air was blowing from the back of the unit and out the front. I only use the dehydrator for making treats for our pets, not that that makes it less important. I've inspected the interior (stainless steel), wiping it with my finger and putting my nose to it. I let it run for an hour afterwards and will wipe it with a damp towel with bicarb tonight. In short, I think by putting a glass cover on the jar, much of the NO2 refluxed back down and/or went straight outside. I understand your concern, but if you saw what I'm talking about you might get my point. In any case using that was a one time thing just to get this batch reacted.
Also, I am planning to do what you say - drop with copper and be done with it. However, the bulk of this thread is talking about the trouble I'm having converting the AgCl to Ag. It's the AgCl, not the AgNO3 that I'm planning to reprocess with lye. I'm using the nitric to separate the silver (good) from the silver chloride (bad).
Now I gotta go find a cheap hot plate.
Lab glass (heat resistant) beakers will work on hot plates and hold up to fire. I have lab beakers that I use. I also have large glass jars from the goodwill to be used to hold my solutions in that I filter and (or) drop my silver or gold with. The Skippy jar would be good for that, not for heating solutions.
I know what type of dehydrator you're talking about. I have a dehydrator, but not the kind you have.
Also, I do use MAPP and propane. But, if I'll get less of a loss with the propane, then I'll start using it for all my silver melts. Propane does melt in the same amount of time as MAPP to me, it's just MAPP gets much hotter.
Kevin
Oh - how the mistakes get repeated... I had a bunch of what I assumed was lightly rinsed silver chloride that dried and stored... after excess NaOH and Sugar... this is what I get... which incidentally will settle to golden liquid and the mix of stuff in it... mostly grey... some black fine (darkening color in this photo). And some whitish specks (silver chloride)zzz
The solution looks alit like a clean gold solution perfectly clear with golden yellow when settled
I guess I have to either blend or waste Nitric?
The solution looks alit like a clean gold solution perfectly clear with golden yellow when settled
I guess I have to either blend or waste Nitric?
