# Made my FIRST batch of silver this evening



## kadriver (Nov 2, 2010)

I started out to make just one batch to get the experience. It turned out so well that I could not stop. I made a total of four batches and ended up with over 11 troy oz of pure (as pure as I could get it) silver.

It there a way to determine the purity that a novice (like me) can perform.

I used the copper cementing method.

Thanks for looking - kadriver


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## Harold_V (Nov 2, 2010)

I would expect your purity to be in the neighborhood of 99%, with the major contaminant being copper. 

If you dissolve one of those items, assuming you have nothing present but silver, and you use the proper amount of nitric, when it is entirely dissolved you should have a solution that is free of color, although it may lean slightly (very light) yellow, or even a hint of very pale green. It is a good idea to bring the solution to a boil, which will liberate traces of brown fumes that tend to linger. 

If you find any color in the solution, that will be a contaminant---most likely to be copper. The solution will have a light green cast (after being boiled) as a result. You can test the solution by withdrawing a drop, which is placed in a spot plate cavity. Add to that drop a drop of ammonium hydroxide. If you have copper present, you'll see a vivid blue color. If you see any particulate matter after dissolution, you likely have a trace of gold present, although it could be some other insoluble substance. The point is, if your silver is pure, there will be no color, and nothing solid left after digestion. 

An assay is the way to determine the purity. 

Harold


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## goldenchild (Nov 2, 2010)

Your silver is beautiful.


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## glondor (Nov 2, 2010)

Your silver is indeed beautiful. I look forward to the day i can get the same results. Can you tell me what you made your first batch from and how you did it?


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## kadriver (Nov 3, 2010)

Here is the process I used to make the silver pictured above:

First of all DON"T DO THIS INSIDE - DO IT OUTDOORS AWAY FROM PEOPLE AND PETS - DON"T BREATH EVEN A TINY WIFF OF THE RED FUMES THAT COME FROM THIS REACTION OR YOU WILL GET SICK!

Preliminary: set up a large plastic tub (available from Lowes in the cement mixing department) with a hot plate sitting in the middle of it. set it up OUTSIDE, do not use your kitchen stove.

I used 130.7 grams of STERLING silver from some old candlestick holders I bought at the flee market.

All the weighted material was removed so only the silver metal remained.

I put this material in an old HEAVY Pyrex glass coffee pot, the kind you can boil liquids in on top of the stove. I bought this off ebay specifically for this purpose. Do not use a regular modern coffee pot from a coffee maker, or it might break and spill acid everywhere.

I calculated the amount of nitric acid to dissolve the amount of silver I was working with (130.7 grams silver). I got several responses about how much acid to use: from 1.2 ml nitric acid per gram of silver to 1.4 ml nitric acid per gram of silver. So I interpolated and used 1.3 ml of nitric acid per gram of silver. So 130.7grams X 1.3ml Nitric = 169.991 or 170 ml nitric acid.

I used a 50/50 mix of water and nitric acid - thanks to a kind input from another member of this forum. Pure nitric acid will work but less efficiently.

First, I measured out 170 ml distilled water and added it to the silver in the coffee pot.

I set the coffee pot with the silver and water in it inside the black tub I got from Lowes next to the hot plate.

Next I put on thick rubber gloves that go all the way to my arm pits protecting my arms, a respirator, and chemical splash goggles (DON"T SKIP THIS STEP).

Then I carefully poured 170 ml Nitric Acid (68% technical grade bought from AtrChemicals.com) into a 250 ml beaker.

I slowly poured the acid into the water-silver mixture that was in the coffee pot then stood back.

The mixture began to react right away billowing red fume.

After about 5 minutes the reaction had slowed a little so I put the blend onto the hot plate set on low. The heat kicked the reaction up a nothch.

In about 10 minutes the reaction had stopped and all but a few tiny pieces were left on the bottom of the coffee pot along with a blue solution with junk floating on top. I should have waited and let the pieces on the bottom completely dissolve, but instead I went to the next step.

I took the coffee pot off the hot plate and set it inside the black tub next to the hot plate. 

I removed the hot plate from the black tub so only the coffee pot was in there.

Next i measured out 11 grams of urea to neutralize some of the remaining nitric acid (I gave a best guess estimate on this amount) . I do not know if this step is necessary, But I know that too much acid in the brew at this point is not good because when we add the copper coil later on to cememnt out the silver, if too much acid is present, the solution will begin to issue red fumes as it dissolves the copper. 

These fumes are not to be taken lightly in any way, They are dangerous and harmful if you breath them. If you breath even a tiny amount you will get sick later on.

I then poured in 340 ml distilled water to dilute the silver nitrate even further. There was already 340 ml of water and acid in the coffee pot. So I increased the amount to 680 ml by adding 340 ml distilled water.

Cooled since adding 340 ml distilled water, I ran the blue solution through a filter flask with a vacuum assist to filter out the trash that was left over from the reaction. There was just under 700 ml of a particle free, pastel blue semi cloudy liquid in the flask. I poured this liquid into a 1000 ml beaker.

I had some old copper wire about 6 foot of 10 gauge copper. I used a broom handle to form a nice coil of copper and bent each end to forms hooks on either end.

I then submerged the copper coil in the liquid and immediately silver began to form on the coil. I would shake the silver off the coil from time to time. I got about 300 ml of fine silver metal on the bottom of the beaker.

After about an hour, the silver quit forming on the coil, so I removed the coil and saved it for later.

I went back to my filtration setup and filtered the silver from the solution. The solution was now crystal clear and deep blue. I poured the filtered liquid into a 2000 ml flask for later processing.

I then took the filter funnel and dumped the silver metal into a white corningware casserole dish and placed it on a hot plate to dry the silver powder.

Once dried, I set up my oxy/acet torch and filled a crucible with the silver powder. I purchased a graphite mold on ebay and used this to make tiny 10 gram loaves of pure silver metal that you see in the picture above.


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## kadriver (Nov 3, 2010)

Here is the silver metal I started with. Sterling Silver candlestick holders with all the weighted material removed.


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## kadriver (Nov 3, 2010)

Here is a filter cart I made up. Plastic cart was $89 at Harbor Freight.

The vacuum pump was $79 from Harbor Freight. It is the kind used to remove air from air conditioning systems.

I used an old air compressor tank ($30 at a yard sale) as a vacuum reservoir. I replaced the compressor with the vacuum pump on top. The vacuum pump sucks on the tank. Then the tank vacuum is used to creat a vacuum on the flask. This serves to isolate the pump from the flask.

If you are going to use this be aware that there is a check valve (allows air flow in one direction only) that must be drilled out. It is located in the tank where the compressor discharges air to the tank. This check valve must be drilled out because it will allow air to go it to the tank (to fill it with air), but it will not allow the vacuum pump to suck air out.

Simply remove the fitting to the air input connection and drill out the check valve with 1/4 inch drill bit.

I also installed a vacuum gauge bought from Harbor Freight. The gauge is an automotive tester for diesels - but works perfectly.

There is a small inline valve between the vacuum reservoir and the filter flask so I can turn the vacuum to the filter flask on and off.


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## kadriver (Nov 3, 2010)

Liquid after first filtering


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## kadriver (Nov 3, 2010)

Pour filtered solution (silver nitrate) into 1000 ml beaker


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## kadriver (Nov 3, 2010)

Copper coil used to cement out the silver


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## kadriver (Nov 3, 2010)

Some of the silver metal in a corningware casserole dish and some cemented silver with copper coil.


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## kadriver (Nov 3, 2010)

Pouring molten silver into a graphite mold. I orderd a 1,2,5,10 ounce bar graphite mold. When it arrived I discovered that I had mistakenly ordered a 1,2,5,10 gram mold.

The 10 gram part worked nice and produced little 10 gram loaves of pure silver metal.

My first few pours were sloppy, Eventually I got the hang of it. I am going to remelt the sloppy pieces and repour so they are all uniform.


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## patnor1011 (Nov 3, 2010)

Very nice post. Thank you for sharing.


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## Buzz (Nov 3, 2010)

I'm trying to find one of those rubber bungs that are used between the flask and Buchner funnel as shown in one of the pictures above. Not had any luck so far.

I'm in the UK but will buy from anywhere.

Can anyone help with a supplier?

Regards
Buzz


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## Barren Realms 007 (Nov 3, 2010)

Buzz said:


> I'm trying to find one of those rubber bungs that are used between the flask and Buchner funnel as shown in one of the pictures above. Not had any luck so far.
> 
> I'm in the UK but will buy from anywhere.
> 
> ...



You could possibly make one with the right material and a little paitence.


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## gold4mike (Nov 3, 2010)

Onlinesciencemall.com sells Buchner funnels and stoppers in all sorts of sizes. I don't know if they sell the stoppers with that large of a hole in them but they sell solid stoppers and a device to make holes in them.


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## Buzz (Nov 3, 2010)

Hi Barren,

I have a home made one but i'm wanting a genuine stopper for my 2 litre flask.
It isn't a perfect fit and using a hand pump to vacate 2 litres is a real pain, as it leaks air.

Thanks for the link Mike, site appears to be down at the moment, i'll try again tomorrow.

Buzz


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## goldsilverpro (Nov 3, 2010)

Buzz said:


> Hi Barren,
> 
> I have a home made one but i'm wanting a genuine stopper for my 2 litre flask.
> It isn't a perfect fit and using a hand pump to vacate 2 litres is a real pain, as it leaks air.
> ...



These rubber adapters fit inside of each other and will fit about anything. 

http://www.sks-science.com/funnels-p-6442.html


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## Barren Realms 007 (Nov 3, 2010)

Buzz said:


> Hi Barren,
> 
> I have a home made one but i'm wanting a genuine stopper for my 2 litre flask.
> It isn't a perfect fit and using a hand pump to vacate 2 litres is a real pain, as it leaks air.
> ...



Put some silicone sealent around it to stop the leaking for a temp fix till you can get the right part.


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## Barren Realms 007 (Nov 3, 2010)

goldsilverpro said:


> Buzz said:
> 
> 
> > Hi Barren,
> ...



Nice link thanks.


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## SilverNitrate (Nov 5, 2010)

Nice bars, a good practice note is to remove the crystals of silver nitrate as much as you can and rinse them off. that way you have less silver nitrate there for your copper to devour. the silver nitrate is simple to turn into silver with sugar.


> I'm trying to find one of those rubber bungs that are used between the flask and Buchner funnel as shown in one of the pictures above. Not had any luck so far.
> 
> I'm in the UK but will buy from anywhere.
> 
> ...


Make sure they are not natural rubber, as the nitric will quickly attack it turning it into a black goo. I can make two of the by carefully cutting the bulb-end of a turkey baster or the bulb-end from a blood-pressure pump. they tend to be made of a soft plastic thats not attacked by the acids.


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## bobbix34 (Feb 1, 2011)

To deplated those items you used to make these fine silver loafs, did you use the HNo3 copper cementing method?


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## Lonnie (Feb 17, 2011)

kadriver 

Very nice !! Congratts I sure wish I was that far along . All I've been able to do with a cell is to make AgCl . I'm going to use your method here and try a small batch just as soon as I can get some good nitric . 

Spent 2 days concentrating battery acid got that done and when mixed with my sodium nitrate I don't get a reaction . No heat no nothing . I bought the Sodium nitrate on ebay and i think they took fertilizer and mixed water with it then filtered the fillers out and dried the rest . 

I think I should have bought the Sodium Nitrate in the little prills or what ever it is they call them and not in the crystal form like I bought . I know I use to make rocket engines and when mixing the A nitrate with water i got a reaction . It got very cold would freeze a dry ice like substance on the outside of the stainless pot . 

Thinking on those lines I took just a little sodium Nitrate ( jerky cure ) and when mixed with the acid I flat got a reaction . A reaction I'm just not getting from this ebay stuff . 

Anyhow nice job and thanks for posting your complete directions in detail . Very helpfull to some of us . 

Lonnie


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## RGJohn (Mar 17, 2011)

The details of the manner in which you produced your silver are very informative and I thank you. I too cemented my silver but my product is not quite so attractive as yours.


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## goldenchild (May 3, 2011)

kadriver said:


> I used 130.7 grams of STERLING silver from some old candlestick holders I bought at the flee market.
> 
> All the weighted material was removed so only the silver metal remained.



Do you remember how much weighted material was removed to come up with the 130 grams? I'm trying to get some rough estimates on weight to silver ratios on candlestick holders. If anyone else can weigh in eghm... it would be much appreciated.

GC


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## metatp (May 3, 2011)

goldenchild said:


> Do you remember how much weighted material was removed to come up with the 130 grams? I'm trying to get some rough estimates on weight to silver ratios on candlestick holders. If anyone else can weigh in eghm... it would be much appreciated.
> GC


If I remember correctly, I got between 20-25g of sterling from one weighted candlestick (I think about 6 inches tall).


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## element47 (May 3, 2011)

goldenchild, I've taken modest numbers of weighted sterling stuff apart. I don't really think a ratio of "net .925" to "gross item weight" is determinable.

At various times, eg; eras of manufacture, the gauges of sterling used will be quite different. I have seen some more recent items where the sterling was about 1 gauge thicker than aluminum foil. Like the thickness of a soda can. You get all done and a 4-5" tall table candleholder might be in the 18-25 gram range. Other items use a nail or an old-style rectangular concrete nail to tie segments of the cementing together. This would make the weighting heavier. Still others use a lot of sand, then seal up the sand with cement. Some multi-candle items will use silver-plated tubing to form stems to multiple candleholders. Those of course yield essentially zero. 

IMO, the best bet is to GROSSLY underestimate the yield when you are buying these items, for your own protection, and pass on them if they are too dear. 

By the way, wear gloves when you take this kind of thing apart, the silver makes scraps that are razor sharp, they can slice the daylights out of your hand(s).


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## metatp (May 3, 2011)

By the way. I would not buy weighted stuff unless you get it really cheap. For buying, I estimate about 12-15g per candlestick. That way, if you gt 25g or more, it is worth the effort to remover the weight. This is especially true if shipping is involved. Very rarely was someone willing to sell as if the recovery was only 15g. They could always get more for their stuff on Ebay.


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## goldenchild (May 4, 2011)

Thanks for the replies. I wish you guys had recorded the weights of those items so I could confirm what I've read. Supposedly about 20% of a weighted piece's mass is the sterling "skin". If this is true then I would use 10% to buy.


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## Harold_V (May 5, 2011)

goldenchild said:


> Thanks for the replies. I wish you guys had recorded the weights of those items so I could confirm what I've read. Supposedly about 20% of a weighted piece's mass is the sterling "skin". If this is true then I would use 10% to buy.


Only a fool would use a formula for buying weighted sterling. I think you'll come to understand that it's the luck of the draw, in spite of your most careful attempts. 

I broke down that kind of material on a regular basis. It was made rosin filled, as well as cement filled. It also had steel reinforcing included, or not. Some times it was a slender piece of steel rod, while other times it was a rather substantial piece. Candle holders, where there was a narrow portion (above the base) was typically reinforced with a rather large piece of steel as compared to the finished diameter. The skin was always thin---they relied on the filling to prevent denting---which failed to work for the most part. 

I'm not suggesting that weighted sterling is not a wise choice---just that it contains only a small percentage of silver. 

Harold


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## Oz (May 5, 2011)

I have one customer that I refine for that can estimate weighted silver accurately. He has bought this type of material for over 30 years and has kept a log book of every manufacturer and part number for each and every piece he has bought over the years. He then deconstructed each piece to have a net sterling weight. In this way he can bid with confidence at auctions for weighted pieces. 

Many would pay much for his hard won data. It makes him the winner at many auctions, I’m just the refiner.


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## jimdoc (May 5, 2011)

Oz said:


> Many would pay much for his hard won data. It makes him the winner at many auctions, I’m just the refiner.



He is a winner even if he loses the auction. Smart man.

Jim


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## metatp (May 5, 2011)

From what I received in the past varied not only in the amount of silver, but the amount of weighted material. That is why I would never use a formula. Percent silver varies more than amount of silver. For a candelstick, I assume no more than 20g of sterling no matter what the total weight. I would also make sure that the base in sterling. Sometime the base is a different material or plastic.


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## goldenchild (May 5, 2011)

HTPatch said:


> From what I received in the past varied not only in the amount of silver, but the amount of weighted material. That is why I would never use a formula. Percent silver varies more than amount of silver. For a candelstick, I assume no more than 20g of sterling no matter what the total weight. I would also make sure that the base in sterling. Sometime the base is a different material or plastic.



Not using a formula is very sound advice! I accuired some weighted material and this is what I found. Believe it or not the amount of sterling out weighed the amount of filler. I really lucked out on this one.

The 2 objects' total weight before processing was 275.8 grams. The sterling came out to be 141.5 grams and the filler came out to be the difference. Some of the filler broke off when I was trying to remove it but not much. There were also 3 little handles that I squeezed out a gram or two of air. You can see one of them in the first picture. 

The bottom sterling that housed the filler was very thin. It reminded me of heavy gauge aluminum foil. But a bit thicker. The tops of the objects were quite thick though. A much heavier guage. I actually needed a pair of sheers to get the initial cuts. The filler was a platic like type of plaster? Very brittle.

(The leading digit on my scale is messed up. Time for a new scale.)


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## metatp (May 5, 2011)

Congratulations! I am guessing it is an older piece. I've had one about 3 inch candle holder that I think was over 300g, with the silver weighing about 22g. There was this cement looking material, but also a very heavy piece of iron in there as well. O did get some salt shaker that were no weighted much, but they were from the early 1900s. I would have kept them, but they had a number of dents.


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## qst42know (May 6, 2011)

> (The leading digit on my scale is messed up. Time for a new scale.)



I have repaired a few LCD displays with a bit of isopropyl alcohol. Often some dirt or oils migrate between the glass and the conductive laminated rubber. There may be better solvents to clean these connections but 90% alcohol has worked for me.


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## goldenchild (May 7, 2011)

qst42know said:


> > (The leading digit on my scale is messed up. Time for a new scale.)
> 
> 
> 
> I have repaired a few LCD displays with a bit of isopropyl alcohol. Often some dirt or oils migrate between the glass and the conductive laminated rubber. There may be better solvents to clean these connections but 90% alcohol has worked for me.



I will definately try this. Thanks for the tip. 8)


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## jmdlcar (May 3, 2012)

kadriver, How pure was the Silver? Thanks Jack


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## kadriver (May 17, 2012)

I really don't have a way to determine the purity of cemented silver.

It is probably around 99% like harold says, but it may be a little higher.

There is no indication of copper in the silver when it goes through my silver cells.

When I cement the silver, I usually pull the copper out before it gets too thin, and before other PMs such as platinum and palladium begin to cement out.

If the copper coil (I use 12 gauge copper wire I bought at a yard sale for - 100ft for $2) is allowed to get too thin, then it begins to break apart leaving small bits of copper in the cemented silver. These bits contaminate the cemented silver, reducing its level of purity. It shows up as blue color in the silver cell. 

I put the pulled, thin copper wire in distilled water in a large 3 liter jar and save it to make copper bars.

I then process the cemented silver by filtering the cemented silver out of the solution (the solution still has much silver) and adding fresh copper wire coils to the remaining solution to fininsh cementing the rest of the silver out of the solution. Other PMs, if present, will also cement out toward the end of the cementing process. These PGMs will get trapped in my silver cell fiters as slimes and saved for processing later on.

To get the purest silver possible in my silver cells, I use the cemented silver that drops in the first few minutes before the copper gets to thin and after the wire gets pulled out, to make anode bars. 

By cementing silver in this way, I believe that the cemented silver is approaching three nines. I know that when I melt the silver that has been cemeted this way, the resulting anode bars are bright and shiney. They look just as bright as the fine silver bars that come from my silver cells.

kadriver


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## jmdlcar (Aug 13, 2012)

Where is a good place to buy Nitric Acid? And where can I buy or get urea to neutralize the acid?

Jack


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## jimdoc (Aug 13, 2012)

jmdlcar said:


> Where is a good place to buy Nitric Acid?



That question seems to be asked at least once a week.



jmdlcar said:


> And where can I buy or get urea to neutralize the acid?
> Jack



You don't need urea.

Jim


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## jmdlcar (Aug 13, 2012)

Thanks. The Nitric Acid I know it been ask. I should have ask if I can find it local will they sell it to anyone? Or should I buy it over the internet to be safe?

Jack


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## jimdoc (Aug 13, 2012)

jmdlcar said:


> Thanks. The Nitric Acid I know it been ask. I should have ask if I can find it local will they sell it to anyone? Or should I buy it over the internet to be safe?
> 
> Jack



You should try to find it local to save on the outrageous hazmat shipping charges.

Different places have different rules or beliefs in whom they should sell to. You would have to check out your area to find out if they will sell it to you, or what their requirements are. 
If it comes down to it then order it on the internet.

Jim


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## jmdlcar (Aug 13, 2012)

I found it here and what do you think?

http://www.ebay.com/itm/Nitric-Acid-70-1-Pint-Grade-Reagent-Gold-Recovery-Stronger-over-sodium-nitrate-/110852000673?pt=LH_DefaultDomain_0&hash=item19cf4b4ba1#ht_2407wt_966

Jack


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## jimdoc (Aug 13, 2012)

jmdlcar said:


> I found it here and what do you think?
> 
> http://www.ebay.com/itm/Nitric-Acid-70-1-Pint-Grade-Reagent-Gold-Recovery-Stronger-over-sodium-nitrate-/110852000673?pt=LH_DefaultDomain_0&hash=item19cf4b4ba1#ht_2407wt_966
> 
> Jack




That is only 1 pint. That works out to about $480 a gallon!

$60 is about what you should expect to pay for 1 gallon, and that is high, and then you would have to add hazmat shipping. I would call around locally if I were you, or check on the internet for a local place.

Jim

Did you see this thread;
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=14844&p=153505&hilit=nitric+acid#p153505


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## 917601 (Sep 1, 2012)

New here, excellent post. Very professional, job well done. Thanks for the step by step pictures.


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## kjt124 (Sep 8, 2012)

I am still sort of datamining the silver section here, but this post was beautifully done and touches on a question I've had stuck in my head since My first or second read through on Hoke...

Hoke suggests using HCl or NaCl on a AgNO3 solution to precipitate out AgCl and then contacting it with Zn or Al in HCl to get clean Ag. How does this method compare with the Cu cementing in terms of expected purity (assuming all appropriate controls) because in term of ease of execution it would seem there is no comparison - drop in your copper and harvest you silver...

Are there particular situations in which either of these methods are particularly strong or weak?

Thoughts?

If this has been directly answered in a thread, I apologize that I have yet to find it. A redirect to the other thread would be appreciated.


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## Smack (Sep 8, 2012)

Copper is the simpler method with minimal contamination from the copper.


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