# My first button finally



## Grelko

It was about time I got around to making my first button.

I've read others posting about how much fun it is to make their first button, but you never actually know exactly HOW MUCH FUN it really is, until you make your first one.  

It has NOT been refined yet. This is just some bonding wires that I panned out after processing chips on my grill.

It came out to 0.8 grams, and definately is not pure. I'm guessing maybe around 14-18k and looks like rose gold, with some borax stuck to it. I added way too much borax and there's still a good bit stuck in the dish along with some tiny gold beads. :lol: But anyways, here it is :mrgreen: (I'm going to take it to the jewelry store one of these days, to see how pure it is before refining it.)








The first of many :mrgreen: 

Now if I can find the time to refining it, along with around 9g of dirty powder from the pins I've processed, I should have a small but shiny "clean" button to show off :lol: (I may keep this tiny button seperate. It IS my first one after all.)


By the way, is borax supposed to increase in size, (like heating up a marshmallow) before it starts to melt? Also, the borax melted black instead of clear, before I even added the gold. Was my flame too hot, or too close to the borax which might have contaminated it with mapp gas fumes etc? It's the 20 Mule Team borax "sodium tetraborate"

Edit - spelling


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## g_axelsson

Congratulations! Now you are really hooked! :mrgreen: 

I was planning to keep my first button but as usual it wasn't that pure. I don't regret refining it again, after all I still have my first gold but now it's so much shinier. On the other hand, it can be a fun thing to keep one ugly button to show how big a difference proper refining can make.

Oh no! I hope I didn't offend you by calling your button ugly... After all, the beauty is in the eyes of the observer. :mrgreen: 

Borax comes in two different versions, hydrated (what you have) and anhydrous borax (also called borax glass). By heating normal borax the water is driven off and it swells up when it leaves as steam as you observed and that is just normal. When the water is driven off it turns into anhydrous borax.
Small amounts of impurities could make the borax take on a color. The borax I use came from a chemical store and melts clear as water without any color. It could also be that your torch deposits some carbon in the borax if it is a reducing flame. As I haven't tested Mule team borax I don't know if it's normal or not.

Göran


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## UncleBenBen

Nice going grelko!

I used the 20 Mule Team and it did swell up as you described. I seem to remember reading that it's from moisture going to steam when heated that causes it, but don't quote me on that.

My mapp torch left some black in my dish too. It was while heating it a bit before my second melt before I put any powder in it.

My torch is close to 20 years old and has been used quite a bit. I took it apart and polished it up before this las melt and must have loosened a bunch of carbon inside it. I put it together and turned on full gas and the normally blue flame ran yellow for a bit. I tapped on it for about 5 minutes with a screwdriver and every tap would put out more carbon and yellow flame. 

But anyways, I'm pretty sure that's what caused mine to discolor. It also seemed to thicken the melted borax a bit. I got some soda ash today to thin it and try to get a few small beads that are stuck in there.


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## MarcoP

Congrats!

I wouldn't take it to the jeweler, I would just refine it again, drop by using a different reducer, melt and weight the difference. Acid test can tell you if it is more the 22k, and it certainly is.

These beads stuck in the borax will probably spoil the result.

Marco


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## Grelko

g_axelsson said:


> Congratulations! Now you are really hooked! :mrgreen:
> 
> Oh no! I hope I didn't offend you by calling your button ugly... After all, the beauty is in the eyes of the observer. :mrgreen:
> 
> Göran



I was already hooked, when I was still watching the videos on Youtube, before I made my account here :lol: (and learned the proper way to do this) Good thing I didn't mess around with the acids etc, until I learned about them on here first.

How DARE you call my button ugly :shock: :lol: :lol: :mrgreen: Don't worry about it haha, it does looks pretty bad on the top. It started out alot worse, it didn't get fully melted and had a chunk of something burnt stuck to it. I think it was tiny pieces of chips that didn't get panned out. I noticed that after dropping it into a glass of water, so I re-melted it.



UncleBenBen said:


> Nice going grelko!
> 
> My mapp torch left some black in my dish too. It was while heating it a bit before my second melt before I put any powder in it.
> 
> I got some soda ash today to thin it and try to get a few small beads that are stuck in there.



I set everything up outside, then I opened the package that the torch came in. It couldn't be carbon from this one, since it was brand new. (Unless there's a glazing on the brand new ones?) The melting dish was never used, so I had to cook out the water, and season it first. That might have done something, or most likely it was the borax itself, but even that was new also. (The borax was probably a little dirty to begin with, since it's the laundry type)

Next time I'll try to heat the borax slower and/or longer, to see if it goes clear.

I read somewhere, that if the gold powder is pure, you can just melt it without needing borax?

I'll need to buy some soda ash, and clean out my melting dish. I have a second one "unopened", that I was going to use for silver, but I can always get more dishes. I wouldn't want to forget in the future and mix dishes, which would contaminate the gold with silver and vice-versa.



MarcoP said:


> Congrats!
> 
> I wouldn't take it to the jeweler, I would just refine it again, drop by using a different reducer, melt and weight the difference. Acid test can tell you if it is more the 22k, and it certainly is.
> 
> These beads stuck in the borax will probably spoil the result.
> 
> Marco



I only wanted to take it to the jeweler to see how well I panned it out. It wasn't actually refined yet. I just took the chips and burnt, crushed, panned, melted them. I tested it with my acids and it passed 18k, but not 22k. (Somewhere between 75% - 91.67% isn't bad for just recovery) The picture seems like it would be over 22k, but in person, it has more of a copper color to it. I even tried to "bite" it, but it wasn't soft/pure enough to leave a mark, for now 8) 

When I get around to refining it, I was going to pound it very thin with a hammer, then toss it into HCL/peroxide until it dissolved, like gold fingers. Then use HCL/CL, rinses, drop with SMB, and re-melt it. Then refine it a second time after that too, if needed.

I may just be able to get away with putting it into solution with HCL/CL, then dropping, but I was thinking about adding it in with the powder I have, from dissolving pins.

I would definately clean out the dish, or use another new one, before melting it again. The tiny beads in the borax are still dirty.

Thank you everyone for all of this wonderful information  I'm also going to give a big thanks to Patnor, because his Processing Chips guide/thread, is where I first read about processing chips. :mrgreen: The pipe+cap with the bar, to crush up the chips, works great.


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## UncleBenBen

That is strange with all your stuff being new. I suppose the manufacturer could apply some type of varnish to protect the brass, but I would think it would burn off pretty quick. It got way too windy here to get the torch and soda ash out yesterday, (my dish is spotted up like a dalmatian!) I'll try it next weekend maybe.

Solid metal will be very slow to digest in HCl/Cl. It took I think about two hours of constant agitation and I lost track of the 5ml bleach additions I used on solid contacts I did a while back. And those were tiny, probably less than 1/32" thick.

You will need to flatten it thin as you can. With the base metals in there it may shatter instead, so do it in a way that will catch all the flying shrapnel! Don't want to lose any after all that work. Then grind it as fine as you can.

Good luck with it Grelko, and stay safe!

Ben


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## Grelko

Just for the fun of it, I took my button down to the jewelry store.

Besides the copper "around 23%" and nickel in it,

Au = 70.21
Ag = 4.83

It came out to being 16.85 Karat

I was a bit suprised, that there was silver in it, since silver isn't as dense as gold, and would have gotten panned out in the process. I'm guessing that it was solder/brazing.

The folks at the jewelry store gave me a big grin, said I should save up a big pile of it, and bring it down :lol: 

They said, that they will buy anything that is 8k or higher.


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## BROKE

I did my first one about a month ago and it came out with a frosty coat on top. I took it and threw it back in AR again and totally dissolved the whole thing and refined it again. I think it took about 24hrs to dissolve back into the AR and dropped it with smb. It came out a heck of alot better. You should give it a try and see how it comes out.

P.s it looks pretty sweet to watch the AR eat away at it.


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## Grelko

BROKE said:


> I did my first one about a month ago and it came out with a frosty coat on top. I took it and threw it back in AR again and totally dissolved the whole thing and refined it again. I think it took about 24hrs to dissolve back into the AR and dropped it with smb. It came out a heck of alot better. You should give it a try and see how it comes out.
> 
> P.s it looks pretty sweet to watch the AR eat away at it.



I saw that while reading your thread, nice work. 

I don't use nitric yet. I was waiting until I buy or make a fume hood/scrubber before I do, since my neighbors live so close. So far, I haven't actually done any "refining". I'm just recovering things slowly for now, using HCL/peroxide, or burning/crushing chips, then panning out bonding wires. I'm still going through alot of material and seperating everything for later.


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## BROKE

When refining my button a 2nd time it did not produce any brown fumes. I put a site glass on my beaker and let it go to town.


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## Shark

I re refined a 6.2 gram button last fall and it took 29 hours to finish it off. Flatten it out or break it into smaller pieces would have speed it up considerably. Here is a real short clip at 28 hours, the button can just be seen bouncing at the front of the container.

https://www.youtube.com/watch?v=gJzg8Ywa2j0


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## Grelko

Shark said:


> I re refined a 6.2 gram button last fall and it took 29 hours to finish it off. Flatten it out or break it into smaller pieces would have speed it up considerably.
> https://www.youtube.com/watch?v=gJzg8Ywa2j0



29 hours isn't bad at all. I don't worry about the time it'll take :lol: I used to make chainmail shirts for the renaissance festival and the one shirt I made for myself took 9 months, a couple hours per day.

It'll might take a few days to fully dissolve, since I'm not using nitric.

I was going to flatten it out as much as I can (trying for 1/2 mm or less) unless it breaks apart first. Then cut it into tiny pieces and put those into HCL/H2O2, "or just CuCl2+ bubbler" to remove the rest of the copper and nickel, filter, rinse, before using HCL/CL, then re-melting it. Basically the same as processing pins.

I just need to remember, that there is a bit of silver in there also. So after evaporating most of the solution when I'm done, the rest will go into a stock pot.


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## BROKE

what are you using to filter your solution?


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## g_axelsson

Grelko said:


> I just need to remember, that there is a bit of silver in there also. So after evaporating most of the solution when I'm done, the rest will go into a stock pot.


I'm curious on how you are reasoning here?

You silver think you will collect in the stockpot, young padawan, Huh?

Sorry, just seen the last Star Wars movie. :mrgreen: 

Göran


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## upcyclist

g_axelsson said:


> Grelko said:
> 
> 
> 
> I just need to remember, that there is a bit of silver in there also. So after evaporating most of the solution when I'm done, the rest will go into a stock pot.
> 
> 
> 
> I'm curious on how you are reasoning here?
> 
> You silver think you will collect in the stockpot, young padawan, Huh?
> 
> Sorry, just seen the last Star Wars movie. :mrgreen:
> 
> Göran
Click to expand...


I'm guessing he's thinking to let them cement out on/with the addition of copper to the stockpot. 

If that's not practical, I need to pay attention, since I was thinking I'd do the same (until I obtain nitric or use Steve's cold nitric recipe). I was going to use a (sort of) no-nitric process for gold for the time being, dissolving most basemetals in HCl, then using HCl+NaNO3 to dissolve the gold for precipitation (skipping the nitric and dropping AgCl with the addition of HCl/NaCl). I thought I'd be okay if the silver went to the stockpot. 

Right now, I'm only processing PMs dropped from old plating solutions, so was hoping HCl would be sufficient since my PMs are already in precipitant form.


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## g_axelsson

upcyclist said:


> g_axelsson said:
> 
> 
> 
> 
> 
> Grelko said:
> 
> 
> 
> I just need to remember, that there is a bit of silver in there also. So after evaporating most of the solution when I'm done, the rest will go into a stock pot.
> 
> 
> 
> I'm curious on how you are reasoning here?
> 
> You silver think you will collect in the stockpot, young padawan, Huh?
> 
> Sorry, just seen the last Star Wars movie. :mrgreen:
> 
> Göran
> 
> Click to expand...
> 
> 
> I'm guessing he's thinking to let them cement out on/with the addition of copper to the stockpot.
> 
> If that's not practical, I need to pay attention, since I was thinking I'd do the same (until I obtain nitric or use Steve's cold nitric recipe). I was going to use a (sort of) no-nitric process for gold for the time being, dissolving most basemetals in HCl, then using HCl+NaNO3 to dissolve the gold for precipitation (skipping the nitric and dropping AgCl with the addition of HCl/NaCl). I thought I'd be okay if the silver went to the stockpot.
> 
> Right now, I'm only processing PMs dropped from old plating solutions, so was hoping HCl would be sufficient since my PMs are already in precipitant form.
Click to expand...

I'm going to put a couple of leading question out, it's better that you find out the answer yourself than I'm just telling you it. This way you have to think a bit for yourself...

Where in the process will the silver be dissolved? Where will it be precipitated? How is it carried along? Where does it end up?

;-) 

Göran


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## Grelko

BROKE said:


> what are you using to filter your solution?



Seeing that I don't have all of the fancy gadgets, that some people in here have, I get to use a good old coffee filter, like I usually do.



g_axelsson said:


> Grelko said:
> 
> 
> 
> I just need to remember, that there is a bit of silver in there also. So after evaporating most of the solution when I'm done, the rest will go into a stock pot.
> 
> 
> 
> I'm curious on how you are reasoning here?
> 
> You silver think you will collect in the stockpot, young padawan, Huh?
> 
> Sorry, just seen the last Star Wars movie. :mrgreen:
> 
> Göran
Click to expand...


Aww man, I want to go see that, but I'm going to need to wait until after christmas. Funds are getting low.



g_axelsson said:


> Where in the process will the silver be dissolved? Where will it be precipitated? How is it carried along? Where does it end up?
> 
> ;-)
> 
> Göran



Don't you love having certain things bookmarked, for just such an occasion :mrgreen: 

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=53&t=2860

(Silver chloride and copper compounds are very hard to eliminate completely from gold. Partly due to the slight solubilities of the compounds in acid medium and partly due to drag down when precipitating. By swinging the pH basic with ammonium hydroxide you can remove the final traces of silver chloride (which is soluble in ammonium hydroxide) that may have tagged along with any residual acid in the gold powder. Copper is also soluble in ammonium hydroxide as well as some other base metal compounds.

There's an old saying an ounce of prevention is worth a pound of cure. It's much easier to clean traces of silver chloride out of the gold powder with a quick hot ammonium hydroxide wash than it is to remove the resulting metallic silver from the melted button. In the long run the small amount of extra effort spent in the wash stage is well worth the purity you will see in the final product.)

So I figure, that once I have the button completely dissolved, I'll add an ammonia wash, before a second refine. Either that, or I get to read more about it :lol:

Edit - I should have just said "Harold's wash" but I've been busy all day and could not remember his name.  http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=325&hilit=pure+shiny


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## jason_recliner

Shark said:


> I re refined a 6.2 gram button last fall and it took 29 hours to finish it off. Flatten it out or break it into smaller pieces would have speed it up considerably. Here is a real short clip at 28 hours, the button can just be seen bouncing at the front of the container.
> 
> https://www.youtube.com/watch?v=gJzg8Ywa2j0


Thanks for posting that, Jeff.
For those of us yet to use nitric, and I expect there are many of us, it's great to see these videos of it in action, with the colours and reactions to expect.


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## UncleBenBen

Grelko, I don't think that's quite what Göran was getting at as far as the traces of silver washed from the gold powder that may make it to your stock pot.

Think more in the way of what happens with the bulk of silver in the button during the refine. Silver's solubility in HCl, when and how it is dealt with...

Hint: We want a crystal clear solution before precipitation right?


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## upcyclist

g_axelsson said:


> Where in the process will the silver be dissolved? Where will it be precipitated? How is it carried along? Where does it end up?



First off, I'm not sure if the question applies to me, Grelko, or both of us, but here's what I planned on doing with the stuff I dropped from the plating solutions:

1. Dropping PMs (and everything else) with zinc dust. Wash precipitate thoroughly to get rid of cyanide compounds before acidifying.
2. Dissolving zinc (and Fe, Sn, Pb, Ni, etc) with HCl. Any silver or gold should stay in the bottom of the beaker in the HCl washing since I'm converting the silver to AgCl and not touching the gold. Waste HCl goes in the stockpot to be sure. To my knowledge, there are no nitrates in this solution, but I believe any free nitrates are grabbed by more active non-PMs (and backing up hope with the stockpot)
3.Then, dissolve the gold in AR (from HCl + the minimum necessary NaN03), filter, and selectively drop the gold with SMB. HCl balance should keep the silver at the bottom and thus in the filter, correct? If not, it too ends up in the stockpot, and would be cemented with copper during the disposal process. 

Nope. Crap. Typing up my process makes me realize that I have no way of knowing if the precip at the bottom in step 3 contains gold or not, unless I add enough nitrate to dissolve it all. 

Ding! Thanks for the leading questions!

Luckily, all I have really done is up through step 2, and have left that precipitate in a jar for later. 

Back to Hoke, and realizing I shouldn't skip the nitric step. I still like #2 though, since I'd rather burn through hydrochloric acid on the zinc than nitric. It remains to be seen whether saving a few bucks is worth the extra steps to thoroughly rinse the precipitant to make sure I'm not making AR when I add nitric (or roasting?). In other words, what takes more time & resources, making cold nitric or rinsing? I'm guessing rinsing, but will try it both ways.


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## UncleBenBen

Why not take a small sample of that precipitant, especially if finely divided, and dissolve a bit in HCl and very little bleach. Heat for a while to gas off chlorine and test with stannous. 

That would tell you pretty quickly what it is and what direction to go in next.


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## Barren Realms 007

upcyclist you might want to do a sample with your cold nitric to make sure you are not making silver chloride that could cause you problems.


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## upcyclist

UncleBenBen said:


> Why not take a small sample of that precipitant, especially if finely divided, and dissolve a bit in HCl and very little bleach. Heat for a while to gas off chlorine and test with stannous.
> 
> That would tell you pretty quickly what it is and what direction to go in next.


Roger that




Barren Realms 007 said:


> upcyclist you might want to do a sample with your cold nitric to make sure you are not making silver chloride that could cause you problems.


If the precipitant is rinsed/roasted (after processing with HCl), and assuming I'm making cold nitric with sulfuric acid, how would chloride get in there? Or do you mean "if not fully rinsed/roasted"?


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## Barren Realms 007

upcyclist said:


> UncleBenBen said:
> 
> 
> 
> Why not take a small sample of that precipitant, especially if finely divided, and dissolve a bit in HCl and very little bleach. Heat for a while to gas off chlorine and test with stannous.
> 
> That would tell you pretty quickly what it is and what direction to go in next.
> 
> 
> 
> Roger that
> 
> 
> 
> 
> Barren Realms 007 said:
> 
> 
> 
> upcyclist you might want to do a sample with your cold nitric to make sure you are not making silver chloride that could cause you problems.
> 
> Click to expand...
> 
> If the precipitant is rinsed/roasted (after processing with HCl), and assuming I'm making cold nitric with sulfuric acid, how would chloride get in there? Or do you mean "if not fully rinsed/roasted"?
Click to expand...


You can have instances of chlorides being present in the nitrates you use that can create the silver chloride. I've had it happen with the Hi-Yield brand of sodium nitrate that I have used so I have made it a practice to only use nitric that I purchase to process silver.


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## g_axelsson

upcyclist said:


> g_axelsson said:
> 
> 
> 
> Where in the process will the silver be dissolved? Where will it be precipitated? How is it carried along? Where does it end up?
> 
> 
> 
> 
> 3.Then, dissolve the gold in AR (from HCl + the minimum necessary NaN03), filter, and selectively drop the gold with SMB. HCl balance should keep the silver at the bottom and thus in the filter, correct? If not, it too ends up in the stockpot, and would be cemented with copper during the disposal process.
Click to expand...

Correct! The silver will form silver chloride and only trace amounts goes into solution, especially if you don't work with super concentrated solutions. It's the high chloride concentration that's dissolves small amounts of silver chloride so it should be diluted with water before final filtration of the gold chloride. The silver carried over to the stock pot is of no economical concern. The bulk silver is caught in the filter.

If you have silver chloride in the stock pot then the bulk of it too is caught in filters if processing the stock pot by chemical way.

(If memory serves me correct then Harold used silver chloride as a collector of values when he processed the stock pot in a furnace. As I understand he added silver chloride to the stock pot via nitrate solutions that also contained PGM:s.
goldrefiningforum.com/phpBB3/viewtopic.php?f=52&t=21273&p=219522#p219522 )

Generally, when processing gold you get the silver in filters or in case of inquarting, in the nitrate solution.

Göran


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## upcyclist

Barren Realms 007 said:


> You can have instances of chlorides being present in the nitrates you use that can create the silver chloride. I've had it happen with the Hi-Yield brand of sodium nitrate that I have used so I have made it a practice to only use nitric that I purchase to process silver.


Ah, that's the exact brand of my cold nitric. Perhaps I can just put my silver aside (keeping it wet) for later for when I can get the good stuff.

Göran, does that mean I'm not off my rocker after all? My problem is knowing when the crap on the bottom is just AgCl and not gold and other metals (i.e., when have I added enough NaNO3 to dissolve the gold?). Should I just stop adding sodium nitrate when I see the apparent amount of my undissolved precipitant stabilize? 

Part of the problem is I'm dealing with a completely unknown amount of gold. I may end up taking uniform samples and running various amounts of sodium nitrate past the precipitant. So, add 5g sodium nitrate to HCl to dissolve gold, filter, dry, weigh; put filtrate back in more HCl and add another 1g sodium nitrate, filter & weigh, etc. I don't know if I have a sensitive enough scale to help figure that one out. The other option is to put in extra nitrate and just suck it up on the amount of SMB I'll need to drop the gold.


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## Barren Realms 007

upcyclist said:


> Barren Realms 007 said:
> 
> 
> 
> You can have instances of chlorides being present in the nitrates you use that can create the silver chloride. I've had it happen with the Hi-Yield brand of sodium nitrate that I have used so I have made it a practice to only use nitric that I purchase to process silver.
> 
> 
> 
> Ah, that's the exact brand of my cold nitric. Perhaps I can just put my silver aside (keeping it wet) for later for when I can get the good stuff.
> 
> Göran, does that mean I'm not off my rocker after all? My problem is knowing when the crap on the bottom is just AgCl and not gold and other metals (i.e., when have I added enough NaNO3 to dissolve the gold?). Should I just stop adding sodium nitrate when I see the apparent amount of my undissolved precipitant stabilize?
> 
> Part of the problem is I'm dealing with a completely unknown amount of gold. I may end up taking uniform samples and running various amounts of sodium nitrate past the precipitant. So, add 5g sodium nitrate to HCl to dissolve gold, filter, dry, weigh; put filtrate back in more HCl and add another 1g sodium nitrate, filter & weigh, etc. I don't know if I have a sensitive enough scale to help figure that one out. The other option is to put in extra nitrate and just suck it up on the amount of SMB I'll need to drop the gold.
Click to expand...


That is something that really only comes with experience. The more you do the more you learn to recognize what the process is doing and how your chemicals together are reacting.


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## upcyclist

Alrighty--good enough. Thanks, as always, for all the help!


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## g_axelsson

upcyclist said:


> Göran, does that mean I'm not off my rocker after all? My problem is knowing when the crap on the bottom is just AgCl and not gold and other metals (i.e., when have I added enough NaNO3 to dissolve the gold?). Should I just stop adding sodium nitrate when I see the apparent amount of my undissolved precipitant stabilize?
> 
> Part of the problem is I'm dealing with a completely unknown amount of gold. I may end up taking uniform samples and running various amounts of sodium nitrate past the precipitant. So, add 5g sodium nitrate to HCl to dissolve gold, filter, dry, weigh; put filtrate back in more HCl and add another 1g sodium nitrate, filter & weigh, etc. I don't know if I have a sensitive enough scale to help figure that one out. The other option is to put in extra nitrate and just suck it up on the amount of SMB I'll need to drop the gold.


To balance the chemicals used is always tricky. If you use too much you create more work denoxing the solution. If you use nitric acid and hydrochloric it's only extra work, while if using cold nitric or poor mans AR it adds extra salts to the mix.

I would start by using less than I think I would need and when it stops reacting, let it settle and decant the majority of solution. Next leach start with more than is needed to get the last part of gold left, if there is any. Test with stannous to see if the amount of dissolved gold is rising or steady.

Then I would filter off the leach from the silver chloride and use that for starting the next batch and do the same thing again, pouring off gold chloride solution when it's stopped working.

At the end I would denox the gold solution, filter and precipitate the gold with SMB. The filters with silver chloride can be processed in many different ways. The solid remains could contain some gold too, left over from the leach, so I would run the silver in a silver cell and any filter from processing the silver ends up in the burn pile.

But this is how I think I would do with what I assume you have. Exactly what you have only you know, what equipment you have, how your lab situation is and what procedures you are comfortable with.
To write down your procedure is a good thing to do, it forces you to think of what will and could happen in each step.

To refine gold is one part doing the chemistry and one part controlling the waste flow to catch any precious metals trying to get away.

Göran


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## Grelko

Well, I had just written out an HUGE explanation that took almost an hour to type out, exactly how I was going to refine my button, using HCL, H2O2, CL, ammonia, tap water, distilled water and SMB, double refining it and of course, Firefox crashes.

So, I'll just say that, after being here since May, reading and re-reading Hokes and many other posts for hours upon hours each day about everything on here, I know what I need to do refine it, I know what items to use, I know how to do it safely, I'm only going to recover/refine the gold and the silver would be going to the stockpot, after removing the rest of the copper and nickel. Then disposing of the left over solutions properly after everything has been tested with stannous.

I hope that I don't seem rude in my response, since the paragraph above this, probably makes me sound like an @%%.

After that, once I get the time to actually do it, I will post a picture of the "clean" button.

I REALLY should have written it out on notepad and had it saved first. It was everything from dissolving the button in HCL/H2O2, silver powder left at the bottom, filter, rinse, HCL/CL, filter, rinse, ammonia wash, drop with SMB, re-refine to catch any traces, testing with stannous, and the solution being clear, then drying the gold powder before melting it without borax, in a new dish. Unless I get a chance to clean out the first dish.

I even had a part added that said how I get frustrated trying to explain things, because I know how it works, but when I say/type it, I always seem forget something, or get way off track. Now I'm even more frustrated because those long 6 paragraphs are gone, but what can ya do :roll: , so it's all good.


----------



## g_axelsson

I still get the feeling that you think silver will remain in solution when you dissolve and precipitate the gold, that you somehow get the silver cementing into the stock pot after the gold is gone.

The bulk of the silver will be caught in the filter before precipitating the gold. I can't see any reason to add the silver chloride to the stock pot unless you plan to use a furnace to treat it. I think it's better to collect the silver chloride and process it separately when you have enough accumulated. It should be stored wet and not be allowed to dry as that will only complicate the treatment later on.

Only trace levels of silver will reach the stock pot as a solution, less than grams per liter of solution. The solubility in NaCl solution gives a indication of how much would be dissolved in the gold chloride. It also shows why cooling and diluting before filtering helps with the silver chloride.
http://www.saltlakemetals.com/Solubility_Of_Silver_Chloride.htm

Göran


----------



## Grelko

g_axelsson said:


> I still get the feeling that you think silver will remain in solution when you dissolve and precipitate the gold, that you somehow get the silver cementing into the stock pot after the gold is gone.
> 
> The bulk of the silver will be caught in the filter before precipitating the gold. I can't see any reason to add the silver chloride to the stock pot unless you plan to use a furnace to treat it. I think it's better to collect the silver chloride and process it separately when you have enough accumulated. It should be stored wet and not be allowed to dry as that will only complicate the treatment later on.
> 
> Only trace levels of silver will reach the stock pot as a solution, less than grams per liter of solution. The solubility in NaCl solution gives a indication of how much would be dissolved in the gold chloride. It also shows why cooling and diluting before filtering helps with the silver chloride.
> http://www.saltlakemetals.com/Solubility_Of_Silver_Chloride.htm
> 
> Göran



I was going to put the silver powder into the stockpot, and not keep it separate, since I was only trying to purify the gold for now. But after reading your reply, I should keep the powder separate, so that it'll be easier to refine, when I start working on it.

How would drying out the silver chloride, complicate treatment later on? (I didn't read up on silver too much yet, since I'm not working with it.) I do know, that you shouldn't let certain types dry out "nitrate+ammonia" because it can become explosive. I started reading all about safety, BEFORE I started reading up on recovery/refining.

I'm going to see if I can explain everything I had written out earlier, in a condensed version.

I know that silver won't dissolve in HCL, but it'll build up an oxidized layer on the outside, so the rest of the material in the button will dissolve, except the silver and gold, leaving both of those in the filter. Except for some trace silver chloride, that will be in solution with the copper and nickel, (maybe gold also if I add too much peroxide) After filtering, rinse etc, out the gold/silver powders, I was going to put the gold into solution with HCL/CL, then filter it, which should leave the silver in the filter, but gold in solution "HAuCl4?, or AuCl3?". 

There may still be traces of silver chloride in solution with the gold, so after dropping it the first time with SMB, I was going to rinse/dry the powders, then wash with ammonia, to remove the silver chloride, since it's soluble in ammonia. Re-refine the gold powder a second time using HCL/CL, and another ammonia rinse, to make sure that I've removed all of the copper, nickel, and silver from the gold.

Also, the ammonia should be hot and I'll need to do a bit of math, but since it's just trace silver chloride being produced, and the button itself only contains around 0.039g, I shouldn't need much more than a couple ml to wash it out. (According to that link)

After testing everything with stannous, I will dispose of most of the solution, and was just going to put the silver powder into a stockpot, because I wasn't really concerned about it for now. Then dry out the gold powder and remelt it without borax in a new dish (unless I get time to clean the first dish) and remelt it, which should be close to .999

I know that I have most likely forgotten to add in a couple steps, using distilled water etc, but I know where those come into play at.

If I am wrong in some of my information, please correct it. Also, thank you for the link, I should be able to read it more later tonight.

Edit - corrected the word separate, because I always misspell it as seperate.


----------



## FrugalRefiner

Grelko said:


> I was going to put the silver powder into the stockpot, and not keep it seperate, since I was only trying to purify the gold for now. But after reading your reply, I should keep the powder seperate, so that it'll be easier to refine, when I start working on it.


In most cases, once you've achieved any separation, it doesn't make sense to recombine them. It would be like sorting through a bunch of coins, separating the pennies, nickels, dimes, etc. into different piles, then putting them all back into the same basket because you were only interested in the quarters. When you become interested in dimes someday, better that they should be in a separate stack.



> How would drying out the silver chloride, complicate treatment later on?


If you let it dry, it forms a very strong crystalline matrix that will make further processing more difficult.



> I know that silver won't dissolve in HCL, but it'll build up an oxidized layer on the outside, so the rest of the material in the button will dissolve, except the silver and gold, leaving both of those in the filter.


The problem is that the layer of silver chloride can bring the reaction to a halt. If there is enough silver in the button (I don't know if there is), it forms an impermeable barrier on the outside, and it prevents the other metals from being dissolved.



> There may still be traces of silver chloride in solution with the gold, so after dropping it the first time with SMB, I was going to rinse/dry the powders, then wash with ammonia, to remove the silver chloride, since it's soluble in ammonia. Re-refine the gold powder a second time using HCL/CL, and another ammonia rinse, to make sure that I've removed all of the copper, nickel, and silver from the gold.


There is no need to dry the precipitate before the ammonia rinse, if that's the process you choose. There are other alternatives. Silver chloride is only slightly soluble in concentrated chloride solution. If you use AR, diluting it prior to precipitation will greatly reduce it. Using HCl/bleach you probably won't have much as the bleach will be diluting and neutralizing the HCl as you go.

Cooling the solution prior to filtering helps too. Silver chloride is more soluble in hot solutions than in cold solutions.

Lou has described a technique for washing the powder with only HCl that also effectively eliminates any silver chloride unless there are large amounts present.

If you choose to use ammonia, be sure to reacidify the resulting ammonia wash solution promptly. Under certain circumstances, it can create explosive compounds.

Keep studying. It takes a while to absorb the fine points.

Dave


----------



## g_axelsson

Dave gave very good advice and answered most of your questions.

I just want to point out a small detail...


Grelko said:


> I know that silver won't dissolve in HCL, but it'll build up an oxidized layer on the outside, so the rest of the material in the button will dissolve, except the silver and gold, leaving both of those in the filter. Except for some trace silver chloride, that will be in solution with the copper and nickel, (maybe gold also if I add too much peroxide) After filtering, rinse etc, out the gold/silver powders, I was going to put the gold into solution with HCL/CL, then filter it, which should leave the silver in the filter, but gold in solution "HAuCl4?, or AuCl3?".


You can't dissolve out any base metals from your button, it has too high gold content. The base metals on the surface might dissolve but the gold will form a protective layer. To be able to dissolve the base metals from the gold you need to mix it with other metals down to 25% gold content. Look up inquarting for that procedure.

In your case I would recommend to dissolve the button right away, the silver content of 5% is close to the limit when it starts to give problem but I think it is low enough to be able to directly dissolve the button. You need to flatten it out very much to be able to dissolve it with HCl + Cl and I think it will take quite some time to do it. As you melted the bond wires into a button you made it a lot harder to refine with HCl + Cl.
Maybe poor mans AR is the easier way to go, just keep the amount of nitric down, you don't need a lot for 0.8g gold. Then a proper denox afterwards (add a few drops of sufuric acid to precipitate lead and making it easier to denox), filtering and precipitating the gold.

Göran


----------



## Grelko

FrugalRefiner said:


> In most cases, once you've achieved any separation, it doesn't make sense to recombine them. It would be like sorting through a bunch of coins, separating the pennies, nickels, dimes, etc. into different piles, then putting them all back into the same basket because you were only interested in the quarters. When you become interested in dimes someday, better that they should be in a separate stack.
> 
> If you let it dry, it forms a very strong crystalline matrix that will make further processing more difficult.
> 
> The problem is that the layer of silver chloride can bring the reaction to a halt. If there is enough silver in the button (I don't know if there is), it forms an impermeable barrier on the outside, and it prevents the other metals from being dissolved.
> 
> There is no need to dry the precipitate before the ammonia rinse, if that's the process you choose. There are other alternatives. Silver chloride is only slightly soluble in concentrated chloride solution. If you use AR, diluting it prior to precipitation will greatly reduce it. Using HCl/bleach you probably won't have much as the bleach will be diluting and neutralizing the HCl as you go.
> 
> Cooling the solution prior to filtering helps too. Silver chloride is more soluble in hot solutions than in cold solutions.
> 
> Lou has described a technique for washing the powder with only HCl that also effectively eliminates any silver chloride unless there are large amounts present.
> 
> If you choose to use ammonia, be sure to reacidify the resulting ammonia wash solution promptly. Under certain circumstances, it can create explosive compounds.
> 
> Keep studying. It takes a while to absorb the fine points.
> 
> Dave



That is exactly what I was going to do, but yes you guys are right. I should keep it separate, instead of trying to take ALL of the silver back out, there will just be a little in the stockpot. (taking out 1 or 2 dimes, instead of a big pile of them) Sometimes a play on words helps :lol: 

I'll have to look up information about that strong crystalline matrix, I haven't read about it yet. That's why I hope, that I didn't sound too much like a know-it-all in my other post, because I still have alot of reading to do.

I really didn't want to start using nitric acid, until I was properly setup for it, so I will be using HCl/Cl.

This is a part that I don't understand. I think that I have it backwards somehow. If I cool the solution, the silver chloride will become less soluble in the ammonia, but I was trying to put it into solution, so that I can just filter out the gold and the silver would remain in the ammonia. I hope I explained this right.

I'll be re-reading the wash technique a few more times to make sure I have it correct. Especially the part about HCl for silver chloride.

I thought that ammonia didn't need to be acidified again, unless you're using nitric acid? I'll read about this more also, since I REALLY don't want to accidently make fulminating silver etc.

I'm always studying on here, and even if I was able to recite it to someone word for word, there is a chance, that I could forget something, so I keep reading it until it's completely absorbed into my memory. :mrgreen: 



g_axelsson said:


> Dave gave very good advice and answered most of your questions.



Absolutely, this helps me alot. It's like learning a new language, it's going to take a couple years to understand most of it.



> Grelko said:
> 
> 
> 
> I know that silver won't dissolve in HCl, but it'll build up an oxidized layer on the outside, so the rest of the material in the button will dissolve, except the silver and gold, leaving both of those in the filter. Except for some trace silver chloride, that will be in solution with the copper and nickel, (maybe gold also if I add too much peroxide) After filtering, rinse etc, out the gold/silver powders, I was going to put the gold into solution with HCL/CL, then filter it, which should leave the silver in the filter, but gold in solution "HAuCl4?, or AuCl3?".
> 
> 
> 
> You can't dissolve out any base metals from your button, it has too high gold content. The base metals on the surface might dissolve but the gold will form a protective layer. To be able to dissolve the base metals from the gold you need to mix it with other metals down to 25% gold content. Look up inquarting for that procedure.
> 
> In your case I would recommend to dissolve the button right away, the silver content of 5% is close to the limit when it starts to give problem but I think it is low enough to be able to directly dissolve the button. You need to flatten it out very much to be able to dissolve it with HCl + Cl and I think it will take quite some time to do it. As you melted the bond wires into a button you made it a lot harder to refine with HCl + Cl.
> Maybe poor mans AR is the easier way to go, just keep the amount of nitric down, you don't need a lot for 0.8g gold. Then a proper denox afterwards (add a few drops of sufuric acid to precipitate lead and making it easier to denox), filtering and precipitating the gold.
> 
> Göran
Click to expand...


I really should have waited :lol:

I was thinking about inquarting it with copper, but I wasn't sure on the "upper limit" of gold or silver in the alloy, before it would become too hard to remove. I thought it was around 18k and the button is at 16.85k, which is why I was hoping to just dissolve the base metals out of it. The gold is 70.21, and the silver is 4.83. 

It wouldn't be too hard to inquart it to get the gold to 25% (24.96%). I would only need around 1.45g of copper, which would also bring the silver down near 1.7% Then I should be able to remove the base metals alot easier this way. I know it'll take a while, but I'm not in any hurry.

In my other post, I was saying that I'm going to try and flatten it to around 1/2 mm and cut it up, but if it breaks first, I'll try to smash the pieces up small as possible before trying to dissolve it.

After I flatten it etc, I was going to use HCl/H2O2, to remove the base metals, but if it'll be easier with HCl/Cl, I'll do that instead. I really didn't want to use any nitric yet. (I'm always saying this, but I know it''d be alot easier, if I just started using it)

I'm not that good on chemical equations yet, but isn't "poor mans AR" something like H2SO4+NaNO3 = Na2SO4+HNO3 (sulfuric acid+sodium nitrate = sodium sulfate with nitric acid as the byproduct)

For some odd reason, I feel alot safer using jewelry testing solution "which is basically AR anyways, except I think it's potassium nitrate" instead of actual AR for now. Is it possible to just dissolve the button with the 22k solution since I wouldn't need much? I have the 10, 14, 18 and 22k testers, but I can't seem to find silver tester around here.

I read about the jewelry tester after I tested a piece of metal, that may have been aluminum and got a tiny red cloud coming off of it, while it fizzed like crazy.

The easiest way to fix this, would be to sell it to the jewelry store, but I'm too stubborn and I like shiny things :mrgreen:

Edit - fixed a few things and spelling errors


----------



## upcyclist

Grelko said:


> I'll have to look up information about that strong crystalline matrix, I haven't read about it yet.


This is why Hoke instructs the reader to keep the silver chloride wet (Hoke, p. 49).



Grelko said:


> After I flatten it etc, I was going to use HCL/H2O2, to remove the base metals, but if it'll be easier with HCL/CL, I'll do that instead. I really didn't want to use any nitric yet. (I'm always saying this, but I know it''d be alot easier, if I just started using it)


If you use HCl/Cl, you'll dissolve pretty much everything including your gold. I believe that means your gold drop will be more apt to carry down other impurities with it. 



Grelko said:


> I'm not that good on chemical equations yet, but isn't "poor mans AR" something like H2SO4+NaNo3 = Na2SO4+HNO3 (sulfuric acid+sodium nitrate = sodium sulfate with nitric acid as the byproduct)


*HCl *+ NaNO3 is *poor man's AR*, because the nitrate molecules act in the same way as those from nitric acid--mixing those with the chloride ions is forming aqua regia. It's a "poor" substitute in that you're introducing a new impurity (sodium) to do so.
*H2SO4*+NaNO3 makes *nitric acid* & sodium sulfate, as you said. _Nitric acid is not poor man's AR_.

On a side note, be careful with your chemical symbols--lowercase _L_ for chlorine (not HCL/CL, but HCl/Cl), uppercase _O_ for oxygen (not NaNo3, but NaNO3). We're all pretty sure you're not talking about Nobellium (hehe), but it'll make it easier for others to follow, and won't confuse or teach bad habits to readers without a lot of chemistry knowledge.


----------



## Grelko

upcyclist said:


> This is why Hoke instructs the reader to keep the silver chloride wet (Hoke, p. 49).
> 
> If you use HCl/Cl, you'll dissolve pretty much everything including your gold. I believe that means your gold drop will be more apt to carry down other impurities with it.
> 
> *H2SO4*+NaNO3 makes *nitric acid* & sodium sulfate, as you said. _Nitric acid is not poor man's AR_.
> 
> On a side note, be careful with your chemical symbols--lowercase _L_ for chlorine (not HCL/CL, but HCl/Cl), uppercase _O_ for oxygen (not NaNo3, but NaNO3). We're all pretty sure you're not talking about Nobellium (hehe), but it'll make it easier for others to follow, and won't confuse or teach bad habits to readers without a lot of chemistry knowledge.



Looks like I'll need to go back and read parts of Hoke's again. :lol:

That's why I was thinking about inquarting the button, then removing the base metals first using HCl/H2O2.

You are correct, I actually meant the equation for making nitric acid, not poor man's AR. I need to remember that "poor man's AR" is HCl+NaNO3 "Hydrochloric acid+sodium nitrate"

Thank you for catching my mistake the chemical symbols, I always seem to capitalize the L for some reason. I'll need to remember this and I've fixed the spelling of it, in my last post.

Also, while responding to this, I learned how to "lower" the numbers when writing out equations like H2O2 using [ sub ] and [ / sub ] to make it H2O2 . So thank you for that also.


----------



## FrugalRefiner

Grelko said:


> Looks like I'll need to go back and read parts of Hoke's again. :lol:


Don't read parts again. Read the whole book again. I've said this before, but I've read the book through at least six times, including a couple times while proofreading every word for the versions in my signature line. I have learned new things every time. 

You don't know what you miss when you miss it.



> Also, while responding to this, I learned how to "lower" the numbers when writing out equations like H2O2 using [ sub ] and [ / sub ] to make it H2O2 . So thank you for that also.


Excellent. Now you can go one step further by making the numbers a smaller size by using the Font size. H2O2 becomes H2O2.

Whether you select the subscript button first, or the Font size control first seems to depend on the browser you're using. I described it in the Chemical Formulas post in the Tips thread.

Dave


----------



## Grelko

FrugalRefiner said:


> Grelko said:
> 
> 
> 
> Looks like I'll need to go back and read parts of Hoke's again. :lol:
> 
> 
> 
> Don't read parts again. Read the whole book again. I've said this before, but I've read the book through at least six times, including a couple times while proofreading every word for the versions in my signature line. I have learned new things every time.
> 
> You don't know what you miss when you miss it.
> 
> 
> 
> 
> Also, while responding to this, I learned how to "lower" the numbers when writing out equations like H2O2 using [ sub ] and [ / sub ] to make it H2O2 . So thank you for that also.
> 
> Click to expand...
> 
> Excellent. Now you can go one step further by making the numbers a smaller size by using the Font size. H2O2 becomes H2O2.
> 
> Whether you select the subscript button first, or the Font size control first seems to depend on the browser you're using. I described it in the Chemical Formulas post in the Tips thread.
> 
> Dave
Click to expand...


I've read the entire book only once so far, but I've gone back to read certain parts atleast fifty times by now. I'll just read the entire thing again, it'll help me remember the parts I already know, even more.

There's a button for it? (I see it up there now :lol I've always just typed everything out.


----------



## upcyclist

FrugalRefiner said:


> Grelko said:
> 
> 
> 
> Also, while responding to this, I learned how to "lower" the numbers when writing out equations like H2O2 using [ sub ] and [ / sub ] to make it H2O2 . So thank you for that also.
> 
> 
> 
> Excellent. Now you can go one step further by making the numbers a smaller size by using the Font size. H2O2 becomes H2O2.
> 
> Whether you select the subscript button first, or the Font size control first seems to depend on the browser you're using. I described it in the Chemical Formulas post in the Tips thread.
Click to expand...

Ah, I hadn't caught that. Good tip!


----------



## Grelko

While I was removing some silver contacts yesterday, I remembered that CuCl2 "AP" can dissolve gold, when peroxide is added. (This is the reason I had to completely dissolve my pins)

I flattened it out to 0.5mm or less and suprisingly it didn't break into pieces. Then I put it into a mason jar filled with approximately 3-1 of HCl/H2O2. I just have it sitting on the ground outside, without a bubbler right now. I didn't tighten the lid. There's about 2 ounces of solution in the jar and the button is 0.8g. I probably didn't need quite that much, but I'm still learning how to create the least amount of waste.

An hour later, I came back to check on it and it's bubbling a little on its own, with a slight yellowish/green to it. 

It's 16.85k, there's 70.21% gold, 4.83% silver, around 23% copper and some nickel in it also. (I repeated these numbers, so I don't have to keep scrolling up)

I'll let it go by itself for a few days, and see how it turns out.


----------



## Grelko

g_axelsson said:


> You can't dissolve out any base metals from your button, it has too high gold content. The base metals on the surface might dissolve but the gold will form a protective layer.
> Göran



I think it has gone as far as it will go, just using HCl+H2O2. Every few days I would add a little peroxide to it, and it's right around 1-1 instead of 3-1 now. The flattened button looks about 50% dissolved and the solution is a darker shade of yellow. There is a tiny bit of powder at the bottom. I haven't tested with stannous yet.

Now that I'm finished with my little experiment, I can get back to cleaning up this button.(It's not that I didn't trust you, it's that I like seeing the different reactions for myself, to learn about it firsthand)

Since the button has been partially dissolved, the percentages of gold and silver would be different. Using HCl+Cl most likely wouldn't work now, so I am going to filter the solution, take the bit of powder and the rest of the button, and inquart it with copper, then pour it into shots/cornflakes.

Take the inquarted flakes, flatten them, or if they're already very small, put them back into the solution that contains the dissolved portion of the button, since this solution would be slightly CuCl2 along with a bubbler. (I shouldn't need to add fresh HCl, unless the solution is too diluted to work from all the H2O2, but I can always evaporate it a little.) 

After bringing the total gold down to 25% or less "adding 1.5g of copper", that will put the silver under 1.7% and should let the button completely dissolve this time.

The copper and nickel should be in solution, silver doesn't get affected much and should drop to the bottom with the gold powder. If any gold is in solution, I will saturate it with copper, which will precipitate it. Test to be sure the solution is negative for gold and proceed from there.

If I learn how to do this the hard way, the easy way will seem alot easier.


----------



## g_axelsson

Nothing beats first hand experience. 8) 

Inquarting with copper chloride etch, that's a first time on this forum I think.

When doing experiments you should have a theory about what is going to happen, then when it doesn't do what you want, go back and find out what really happened and learn from that. Maybe it's a simple detail that slipped your mind or a major error in your knowledge.

When it works as planned then you can feel proud that you made it and go on with the next experiment. That's progress.

Göran


----------



## Grelko

g_axelsson said:


> Nothing beats first hand experience. 8)
> 
> Inquarting with copper chloride etch, that's a first time on this forum I think.
> 
> When doing experiments you should have a theory about what is going to happen, then when it doesn't do what you want, go back and find out what really happened and learn from that. Maybe it's a simple detail that slipped your mind or a major error in your knowledge.
> 
> When it works as planned then you can feel proud that you made it and go on with the next experiment. That's progress.
> 
> Göran



I was thinking, that since the button wouldn't completely dissolve because of all of the gold/silver in it, If I dissolved the top layer off with HCl+H2O2, it would put some of the copper, nickel, and possibly gold into solution. The copper would make it slightly CuCl2 and I could use it afterwards, instead of having extra waste to deal with at the end. 

Plus, because I'm using copper to inquart, I can use CuCl2 "AP" solution to dissolve it, without having to use nitric.


----------



## g_axelsson

I can't see why it wouldn't work to inquart with copper and CuCl2, it will even dissolve palladium. But it will take quite a while I think but the thinner it is the faster it will dissolve.

I would still dissolve the gold afterwards for a final refining.

Göran


----------



## Grelko

g_axelsson said:


> I can't see why it wouldn't work to inquart with copper and CuCl2, it will even dissolve palladium. But it will take quite a while I think but the thinner it is the faster it will dissolve.
> 
> I would still dissolve the gold afterwards for a final refining.
> 
> Göran



Inquarting with copper chloride etch, is on the forum already, sort of. If you search "inquarting copper" there's some links, but they're mainly talking about karat jewelry and how it'll take 4 times the amount of nitric to dissolve copper, than it does silver etc.

I don't mind waiting, I have enough things to take apart, read on here and everything else to do while it's dissolving.

I was going to put the powder in HCl+Cl and do all of the rinses and possibly a second refining with HCl+Cl afterwards if it looks cloudy or off colored. I'm seeing if I can get .999 with this first button.

Edit - switched inquart copper, to inquarting copper, for the search. There are more results.


----------



## UncleBenBen

Grelko, I can't help but think you are driving all the way around the block to get to the house next door.

You're gold content should be high enough that you shouldn't need to inquart. Try adding a few ml's of bleach at a time to the solution you have it in now. If you got it that thin I would think it should work to dissolve the gold. The silver should be left as its chloride to be filtered out. Yes you would have base metals left in solution with the gold but A LOT less would follow it this time, the majority of which could washed out of the powder.


----------



## Grelko

g_axelsson said:


> it will even dissolve palladium.



So, if I had a button that has Pd, Au, Cu, and Ni in it, I could use CuCl2 and it would dissolve the Pd, Cu, and Ni, leaving the Au as powder, "since Au wouldn't be dissolved much unless you add H2O2, or a bubbler". Filter, then saturate the solution with Cu, precipitating the Pd as powder, since Ni stays in solution. The Pd would have traces left in it though.

Edit - reworded

Basically it would be like partially refining the left over "stockpot solution" at the same time as recovering gold, before the left over solution actually goes into the stockpot? Or am I going off track with this?


----------



## Grelko

UncleBenBen said:


> Grelko, I can't help but think you are driving all the way around the block to get to the house next door.
> 
> You're gold content should be high enough that you shouldn't need to inquart. Try adding a few ml's of bleach at a time to the solution you have it in now. If you got it that thin I would think it should work to dissolve the gold. The silver should be left as its chloride to be filtered out. Yes you would have base metals left in solution with the gold but A LOT less would follow it this time, the majority of which could washed out of the powder.



I can always try this first, and by the off chance it didn't fully dissolve, I'd go with inquarting. A second refining after that would finish cleaning everything up.


----------



## UncleBenBen

Good deal!
That's exactly how I was thinking that it couldn't hurt but try. Watch that Cl2 gas! Don't take but the slightest whiff to make one avoid it like the plague.

Good luck Grelko!


----------



## Grelko

UncleBenBen said:


> Good deal!
> That's exactly how I was thinking that it couldn't hurt but try. Watch that Cl2 gas! Don't take but the slightest whiff to make one avoid it like the plague.
> 
> Good luck Grelko!



I have a respirator specifically for Cl gas, since I knew that eventually I would be mixing HCl+Cl. I didn't want to mix it until I actually needed to, since my neighbors live real close, but it's only 0.8g for the button, which would be a couple ml's of CL. I'll just wait for a windy day, or do it through the night etc. I could go up into the woods if I need to, but I've read different threads that say it should be ok to make small amounts. I'm still going to be cautious though.

Since I'm working on this in a mason jar, I could just put the lid on loose, or a plate, sheet of glass etc, and let the Cl gas escape slowly.


----------



## g_axelsson

Thinking about it a bit more I see some problem with copper chloride etch and inquarting.



Grelko said:


> g_axelsson said:
> 
> 
> 
> I can't see why it wouldn't work to inquart with copper and CuCl2, it will even dissolve palladium. But it will take quite a while I think but the thinner it is the faster it will dissolve.
> 
> I would still dissolve the gold afterwards for a final refining.
> 
> Göran
> 
> 
> 
> 
> Inquarting with copper chloride etch, is on the forum already, sort of. If you search "inquarting copper" there's some links, but they're mainly talking about karat jewelry and how it'll take 4 times the amount of nitric to dissolve copper, than it does silver etc.
> 
> I don't mind waiting, I have enough things to take apart, read on here and everything else to do while it's dissolving.
> 
> I was going to put the powder in HCl+Cl and do all of the rinses and possibly a second refining with HCl+Cl afterwards if it looks cloudy or off colored. I'm seeing if I can get .999 with this first button.
> 
> Edit - switched inquart copper, to inquarting copper, for the search. There are more results.
Click to expand...

Not inquarting with copper, that's well known and except from the extra nitric consumption it doesn't add any complications.

To use copper chloride etch in an inquartion on the other hand is quite different. I think it will take a lot longer. With nitric acid you get gas evolution where the etch is going on and will move liquid in and out of the inquarted metal. With copper chloride you will convert copper II chloride into copper I chloride inside the metal and if the concentration is too high it will precipitate copper I chloride on the inside and it will be really hard to get that into solution again. Thinking of it I would recommend using a lot more than 75% copper, more like 90% or more so the gold would just fall off as a black mud. This is not what you would get with normal inquartion, then you get brown clumps that keeps together and are easy to work with, the fine black mud will be really annoying as it will easily move with the liquid and take a long time to settle.

If you have access to nitric use that instead and just dissolve the button. If you don't have access to nitric acid, get some sodium or potassium nitrate salt and try poor mans AR.

Once you gone nitric you never go back.

Göran


----------



## Grelko

g_axelsson said:


> To use copper chloride etch in an inquartion on the other hand is quite different. I think it will take a lot longer. With nitric acid you get gas evolution where the etch is going on and will move liquid in and out of the inquarted metal. With copper chloride you will convert copper II chloride into copper I chloride inside the metal and if the concentration is too high it will precipitate copper I chloride on the inside and it will be really hard to get that into solution again. Thinking of it I would recommend using a lot more than 75% copper, more like 90% or more so the gold would just fall off as a black mud. This is not what you would get with normal inquartion, then you get brown clumps that keeps together and are easy to work with, the fine black mud will be really annoying as it will easily move with the liquid and take a long time to settle.
> Göran



I was going to start off trying HCl+Cl and see how that went. If it doesn't fully dissolve the button, I might experiment a bit with the copper chloride etch, or just give in and see if I can make a small amount of "poor man's"

I didn't think it could convert to copper I chloride inside the metal, since I'd have a bubbler running. Even with 90% copper, I wouldn't need to add much to the button. I figured it would be more like dissolving a large pin. (I need to read more about alloys) Even if the fine mud takes a long time to settle, I could just filter it, while it's still floating around the solution.

So many ideas for experiments, no room for a decent lab setup.

This made me wonder about a "nickel" inquart. (I've read about someone inquarting with zinc also) You could use HCl+H2O2 to dissolve the nickel and copper, which should drop the gold and silver as powder. Just make sure you have enough solution to hold the nickel and copper chlorides, or the copper would precipitate.

Or even use ferric chloride to dissolve the nickel http://lanthanumkchemistry.over-blog.com/article-the-dissolving-of-nickel-101259615.html


----------



## solar_plasma

Just as a side note, it was difficult (at least to me) to understand what was discussed here. "Inquarting with CuCl2" might be confusing. In order to make it more clear:

*inquarting *is the alloying step (1/4 gold), while the next step wherein the base metals and silver are dissolved by nitric acid is called *parting* (parting silver from gold).

So you are normally *inquarting *with silver or copper . You are *parting *(normally) with nitric.

What you guys call "inquarting", the hole two step process, is called "*parting by the quart*" [this line I edited after I found evidence for what I wrote]


----------



## Grelko

solar_plasma said:


> Just as a side note, it was difficult (at least to me) to understand what was discussed here. "Inquarting with CuCl2" might be confusing. In order to make it more clear:
> 
> *inquarting *is the alloying step, while the next step wherein the base metals silver are dissolved by nitric acid is called *parting*.
> 
> So you are normally *inquarting *with silver or copper . You are *parting *(normally) with nitric.
> 
> If this difference only exists in german language and not in english, please correst me.



I hope that this explains it better.

I was going to inquart with copper, so that my button is under 25% gold and under 2% silver. Then I would place the button "that is mostly copper" into CuCl2, to dissolve the copper out of the button, which should leave the gold and silver, at the bottom as powder. I wasn't going to use nitric for this.

I am *inquarting* with copper. I am *parting* with CuCl2 (AP)

I have decided to try HCl+Cl, to see if that will fully dissolve the button first.


----------



## solar_plasma

With this small silver content I would not inquart but use straight AR instead. Inqarting is used, when the silver content is too high to get the gold alloy dissolved in AR. AR is able to hold small ammounts of silver in solution in the scape of complexes, which get insoluble AgCl as soon as the solution is getting dilluted.


----------



## Grelko

solar_plasma said:


> With this small silver content I would not inquart but use straight AR instead. Inqarting is used, when the silver content is too high to get the gold alloy dissolved in AR. AR is able to hold small ammounts of silver in solution in the scape of complexes, which get insoluble AgCl as soon as the solution is getting dilluted.



I was trying to figure out a "work around", so that I didn't need to use nitric in the first place. I might try to make poorman's AR sometime, if I can find a store that carries Hi Yield etc, or even a store that makes sausage should carry sodium nitrate.

By any chance, would jewelry testing solution (18 or 22k) work like AR to dissolve this? I almost never test jewelry anymore.


----------



## solar_plasma

I think this is kind of like to say: I want to repair my car, but since I have no tools I am trying to find a workaround with my swiss army knive.

Better stick to material you can refine with the tools you have. This might not be correct in your case, but in most cases it is, - probably also in yours.


----------



## g_axelsson

Thanks Björn for putting us on the straight part... or parting. 

Parting is such a sweet sorrow... Finally I understand that Shakespear quote! :mrgreen: 

For poor mans AR you only need a gram or two of nitrate salt. Maybe this would be enough.
http://www.ebay.com/itm/Technical-grade-Sodium-Nitrate-/291648476382?hash=item43e79a94de:g:ZM4AAOSwUdlWgZDd

Göran


----------



## g_axelsson

Grelko said:


> I didn't think it could convert to copper I chloride inside the metal, since I'd have a bubbler running. Even with 90% copper, I wouldn't need to add much to the button. I figured it would be more like dissolving a large pin. (I need to read more about alloys) Even if the fine mud takes a long time to settle, I could just filter it, while it's still floating around the solution.


If you inquart the gold to 8k it will create a porous mass of gold when the copper is dissolved away. The CuCl2 and a Cu turns into two CuCl when they physically meet and after a while the only place with metallic copper is inside the porous mass of gold.

When you dissolve pins you have larger voids so the liquid can easier move through the pin and you don't have the same problem with local saturation.

If you add more copper the gold will break down into a fine mud and you don't have the same problem with local saturation.

Göran


----------



## Grelko

solar_plasma said:


> I think this is kind of like to say: I want to repair my car, but since I have no tools I am trying to find a workaround with my swiss army knive.
> 
> Better stick to material you can refine with the tools you have. This might not be correct in your case, but in most cases it is, - probably also in yours.



That's a good way to explain it, but you wouldn't believe how many things I've fixed over the years without having the proper tool for the job :lol: 

This is why I was trying to figure out a way, that I could remove the base metals, and the silver from my button, by adding more copper, so that I could just use CuCl2 "with all of the other steps" and not need to worry about nitric yet. I was trying to wait until I bought or made a fumehood, before I started using it. 

Some other reasons I haven't used it yet would be, I basically live in the middle of town, my neighbors live about 15 feet away, I have outside pets, and my nieces come over alot, I don't know the laws in my area regarding the use of nitric, and other things.

This is just a hobby for now, so I'm not worried how long it might take. Plus, I'm learning alot while I do all of this. (I never had chemistry in school.)


----------



## Grelko

g_axelsson said:


> For poor mans AR you only need a gram or two of nitrate salt. Maybe this would be enough.
> http://www.ebay.com/itm/Technical-grade-Sodium-Nitrate-/291648476382?hash=item43e79a94de:g:ZM4AAOSwUdlWgZDdGöran



I'd rather not get certain materials shipped to my house, since I don't know the laws in my area yet. I may be able to find sodium nitrate at a farm supply store around here, if I did decide to make a small amount sometime.



g_axelsson said:


> If you inquart the gold to 8k it will create a porous mass of gold when the copper is dissolved away. The CuCl2 and a Cu turns into two CuCl when they physically meet and after a while the only place with metallic copper is inside the porous mass of gold.
> 
> If you add more copper the gold will break down into a fine mud and you don't have the same problem with local saturation.
> 
> Göran



That actually explains alot. So the bond between the CuCl2 is broken, when it touches another atom of Cu, because an electron transfers from the CuCl2 atom to the Cu atom, which turns both of them into CuCl? I WILL learn chemistry eventually :mrgreen:
CuCl2 + Cu > 2 CuCl, without any by-product. 

If the HCl+Cl doesn't work as planned, I'll add enough copper to make it 90% or higher, and see how that works with CuCl2.


Edit - Thank you everyone for taking the time to help me out with this. I know I might be a pain when I start to get off track and ramble on about things "especially when I'm tired, but that's when I get alot of ideas". I won't make random alloys, unless I'm sure that I want to. :lol:


----------



## UncleBenBen

Grelko said:


> I could go up into the woods if I need to,



The first time I put bleach in HCl, I did just that. Worried about the giant green cloud I was about to make. To my surprise it wasn't that bad at all.

I like using a small syringe to make the bleach additions. It makes it easy to keep it at 1 or 2 ml's at a time. In a small amount of solution, with ample time to react between additions, the chlorine output will be minimal.
But definitely do it when and where makes you the most comfortable.


----------



## Grelko

UncleBenBen said:


> Grelko said:
> 
> 
> 
> I could go up into the woods if I need to,
> 
> 
> 
> 
> The first time I put bleach in HCl, I did just that. Worried about the giant green cloud I was about to make. To my surprise it wasn't that bad at all.
> 
> I like using a small syringe to make the bleach additions. It makes it easy to keep it at 1 or 2 ml's at a time. In a small amount of solution, with ample time to react between additions, the chlorine output will be minimal.
> But definitely do it when and where makes you the most comfortable.
Click to expand...


Hmm, I've never read about, or saw a video where HCL+CL produced a green cloud, I'll have to check into that more. I like knowing as much about a process as much as I can, sight, smell, total amount needed etc. It's just that, I didn't expect silver to be in this button when I melted it, (I just wanted to make that first button :lol: ) so I wasn't ready for that part.

I was going to use a dropper bottle, when mixing in the bleach, so that I can make as little fumes as possible. I should be able to do this out behind the garage when the wind is blowing. If I really had to go up into the woods, I'd have to drive a couple miles, with my solutions in the bed of my truck, on pothole filled roads. Not a great idea.

Edit - I found a little information about the green cloud/fumes

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=60&t=1511


Irons said:


> If you can see the green Chlorine gas, don't add any more bleach until it all goes into solution.



Also, if you do a search for "green gas" you'll find more links.


----------



## jason_recliner

Grelko said:


> ... or even a store that makes sausage should carry sodium nitrate.


Pay very close attention to the spelling, as they would likely carry sodium nitrite.
Minor spelling difference, 'wurst' possible result.


----------



## Grelko

jason_recliner said:


> Grelko said:
> 
> 
> 
> ... or even a store that makes sausage should carry sodium nitrate.
> 
> 
> 
> Pay very close attention to the spelling, as they would likely carry sodium nitrite.
> Minor spelling difference, 'wurst' possible result.
Click to expand...


I'll have to find some "links" to see exactly which kind they use. If I used the wrong "ingredient", it could turn out to be a "recipe" for disaster.

Edit - https://en.wikipedia.org/wiki/Sausage_making

Apparently, you are able to use any of the 4. Sodium nitrate/nitrite, or potassium nitrate/nitrite. I'll have to check a couple stores, to see which type they carry. I'll make sure to get the Nitrate type, when I get to that point.


----------



## upcyclist

jason_recliner said:


> Grelko said:
> 
> 
> 
> ... or even a store that makes sausage should carry sodium nitrate.
> 
> 
> 
> Pay very close attention to the spelling, as they would likely carry sodium nitrite.
> Minor spelling difference, 'wurst' possible result.
Click to expand...

Lawdy, that hurt. Well played


----------



## Grelko

upcyclist said:


> jason_recliner said:
> 
> 
> 
> 
> 
> Grelko said:
> 
> 
> 
> ... or even a store that makes sausage should carry sodium nitrate.
> 
> 
> 
> Pay very close attention to the spelling, as they would likely carry sodium nitrite.
> Minor spelling difference, 'wurst' possible result.
> 
> Click to expand...
> 
> Lawdy, that hurt. Well played
Click to expand...


I thought so too, but I may have gone a bit overboard with my response to it.


----------



## UncleBenBen

Nah, I wouldn't say it was overboard.
The quote in your sig line set to the tune of 'spoonful of sugar' just may come close though!

Just messing Grelko, I think it's right clever!


----------



## Grelko

UncleBenBen said:


> Nah, I wouldn't say it was overboard.
> The quote in your sig line set to the tune of 'spoonful of sugar' just may come close though!
> 
> Just messing Grelko, I think it's right clever!



It's easier for me to remember certain things in song form. :mrgreen:


----------



## Grelko

I finally got around to using HCl+Cl on my flattened button. It was approximately 38F (3C) outside when I did this about 2 hours ago.

This is the first time that I've done this step, so I'm taking it very slow.

The original jar has the HCl+H2O2 and some of the button dissolved into it.

I put the button into a new mason jar, then added 150 ml of HCL and used a dropper bottle to slowly add 5 ml of CL. There wasn't any initial reaction, so I stirred it up with a plastic spoon, nothing happened. I transferred the solution to a small ceramic pot, then put it on my hot plate and turned it on low. I let it warm up until it barely began to steam, then shut off the hotplate and let it cool back down, still nothing happened. (I put a flash light up to the solution and didn't see any bubbles)

I thought that the Cl might have left the solution from heating it, so I added another 5 ml to the solution and stirred it again. It starts raining :lol: , so I transferred the solution back into the mason jar and put the lid on loose. It started pouring rain :roll: :lol: , so I figured I would just let the solution work on its own until the rain stopped.

About 30 minutes later it stopped raining, so I went back outside to check on the solution, and it looks like there's a couple small bubbles floating on top, the solution looks a bit more yellow/green and has what appears to be a tiny amount of light grey/white powder at the bottom. I believe this is either silver chloride or salt, so I guess it's working now? :mrgreen:

I'm not in any hurry to finish this, so I was thinking that I might add 5 ml of CL to the solution a few times throughout the day, for the next couple days, until the button is completely dissolved.

I haven't diluted the solution, except for some water that I used to rinse the spoon off with a couple times.

I haven't checked anything with stannous yet, but I'll do that tomorrow.

Edit - reworded


----------



## Grelko

This should speed things up a little.

I took the button out of the HCl/Cl, rinsed it off with water, dried it, then sat down for about 15 minutes with a pair of micro wire cutters. I cut it into probably 200+ pieces, then put it back into the jar, added another 5 ml of "new" CL to it and stirred it up. I put the lid back on loosely, so it doesn't build up pressure.

I still haven't tested anything with stannous. I'm just going to wait until the button is dissolved first.

The old Cl only had 3% of NaClO "sodium hypochlorite" and was atleast 8 months old, so I got a new jug of it which has 8.25%.

Edit - spelling


----------



## Grelko

UncleBenBen said:


> Try adding a few ml's of bleach at a time to the solution you have it in now. If you got it that thin I would think it should work to dissolve the gold. The silver should be left as its chloride to be filtered out.



So far so good. Everything looks dissolved except a tiny bit of grey powdery fluff in the bottom "looks like tiny pieces of a cotton ball" which should be the silver chloride. Also, there's a little piece of what I think is part of the crucible? It looks plastic/ceramic and completely white.

The solution is mainly a light shade of yellow, with a hint of green. I was going to see if I can filter it tomorrow, maybe precipitate and also make another small batch of stannous, since the batch I made a while ago went bad.

Edit - I'll try to get a couple pictures up one of these days.



UncleBenBen said:


> Watch that Cl2 gas! Don't take but the slightest whiff to make one avoid it like the plague.



I had to find out just so I know what it smells like. Atleast this time I used the "wafting technique", instead of sniffing that jug of HCL at the begining of my other thread. To me, besides the regular smell of HCL and Bleach, it smells like very strong concentrated turpentine or some type of floor wax. (It actually reminded me of a roller skating rink I went to when I was little. Maybe the owner was a refiner?) Didn't make me cough, but I barely even got a whiff of it from a couple feet away. Then again, if you do scrap metal, the smell of rotten meat coming from an old refrigerator might be worse.


----------



## UncleBenBen

Nice going with the dissolve Grelko!



Grelko said:


> I cut it into probably 200+ pieces,


You've definitely got something I need to work on...patience. The older I get the less I have!

That piece of white plastic/ceramic could just be something that fell in when you weren't looking. A few months ago I had a beaker containing the decanted solution and washes from a small gold drop that I was going to sit aside and let settle. I sat it on a table by the back door while I went in to get a watch glass. When I got back there were 3 small strings of tiny bubbles rising from the bottom. I stood watching thinking what in the world is in my beaker. Then the breeze picked up and 2 more strings of bubbles started at the top and slowly sank to the bottom.

That's when I noticed the shroud on the aluminum light fixture directly overhead was loose and flaking off tiny bits of Al into the solution! It was pretty neat to watch, should've taken a picture.

But anyway, good job. Keep us updated!

Ben


----------



## Grelko

UncleBenBen said:


> Nice going with the dissolve Grelko!
> 
> 
> 
> Grelko said:
> 
> 
> 
> I cut it into probably 200+ pieces,
> 
> 
> 
> You've definitely got something I need to work on...patience. The older I get the less I have!
Click to expand...


I seem to have more patience as time goes on. The only way I can explain it is with a quote from the first page of this thread.


Grelko said:


> I used to make chainmail shirts for the renaissance festival and the one shirt I made for myself took 9 months, a couple hours per day.






UncleBenBen said:


> That piece of white plastic/ceramic could just be something that fell in when you weren't looking.
> 
> That's when I noticed the shroud on the aluminum light fixture directly overhead was loose and flaking off tiny bits of Al into the solution! It was pretty neat to watch, should've taken a picture.
> 
> But anyway, good job. Keep us updated!
> 
> Ben



It turned out to be a piece of the plastic/wax seal from the inside of the mason jar lid. I had to use a metal lid this time, since my jars with plastic lids are a different size, and have used CuCl2 "A/P" in them.

I didn't think anything fell in since the only time I would have the lid off, was for a couple seconds to add 5-10 mls of CL to it, then it'd put it back on loosley.

It's always fun watching certain reactions like that. :lol: I must have had a small piece of aluminum in my bucket when I processed pins a while back. It looked like a tiny speed boat fizzing its way around the top of the solution.

--------------------------------------

I got around to making a new batch of stannous. (approximately 2.1g tin fishing weights and 20ml HCl) Also found a store nearby that carries pipettes. "Bought 4 of them for now"

Two of my unused plastic funnels decided to make a break for it, they're probably behind the work bench.

I added the first jar that had a small amount of the dissolved button in it, to the second jar which has the rest of the dissolved button. I filtered out the solution through 3x coffee filters and rinsed it down with tap water. 

Anything that was left in the filters, plus the filters themselves, were put into a separate jar for silver, with some water to keep it wet, so the silver chloride doesn't dry out and form that "strong crystalline matrix".

It's pretty cold outside, so I think that I got most of the silver chloride in the filter (less soluable when it's cold). I'll be doing rinses and re-refining it anyways after I precipitate it this first time.

I tested the solution with my new batch of stannous and it was negative (I sat there thinking, I know it's in there, I watched myself put it in there and saw it slowly dissolving over the last week.) It was only a couple minutes since I made the stannous :roll: I waited about 20 minutes to let the tin dissolve and re-tested it. Looks purple to me :mrgreen:

I'll try to get a picture of it up before I precipitate.


----------



## Grelko

I need to buy more gloves, so I won't be precipitating yet. I did get around to taking a couple pictures though.

This should be around 0.5 gram in a 32 ounce "quart" jar. I need to work on using less solution next time.


----------



## jason_recliner

That looks quite dilute, though you can always evaporate it down a little if you like.

But I highly recommend you perform your precipitation in a straight sided jar with no lip, and perfectly smooth insides. Or preferably new, clean beaker, dedicated to the task. Gold powder is stubbornly difficult to remove completely from a lipped jar. It's far easier to use a spray bottle to flush out the last of your solution into said beaker, than it is to flush out precipitated powder.

Also, and I don't mean to offend, see your minor yellow spill in the paper towel's indent from the jar? You can actually add a drop of stannous into that to confirm your reaction, rather than extract more into your spoon. With 1g/litre concentration, this is not so much of a loss. But you will soon learn to work with more concentrated solutions, so you will watch your wastage more closely.

Finally, 1g/litre is an ideal concentration to keep a tiny bottle (say 5 to 15ml) of known gold solution, for positive confirmation of your future testing solutions.

Well done Grelko, you're making good progress.


----------



## Grelko

jason_recliner said:


> That looks quite dilute, though you can always evaporate it down a little if you like.
> 
> But I highly recommend you perform your precipitation in a straight sided jar with no lip, and perfectly smooth insides. Or preferably new, clean beaker, dedicated to the task.
> 
> Also, and I don't mean to offend, see your minor yellow spill in the paper towel's indent from the jar? You can actually add a drop of stannous into that to confirm your reaction, rather than extract more into your spoon.
> 
> But you will soon learn to work with more concentrated solutions, so you will watch your wastage more closely.
> 
> Finally, 1g/litre is an ideal concentration to keep a tiny bottle (say 5 to 15ml) of known gold solution




I was going to slowly evaporate the solution to 50%, unless that would start pushing gold out. It's probably half water by now, so it should be ok.

If I can't find a good enough jar, vase, or "drinking" glass, I might just order a beaker. (The drinking glass wouldn't be used for anything else.)

No offense taken, I'm still learning. I didn't actually notice the yellow on the paper towel, until I had a few drops in the spoon. I've seen people using a white piece of paper, or even white ceramic to test with. (I should have just used 1 drop of solution and 1 drop of stannous, but it was more like 5 of each.)

I read about the concentrated solutions before. There was a thread where someone figured out that EACH DROP of solution they had, was worth around $0.25, so you really wouldn't want to lose any.

I was going to keep some in a dropper bottle after evaporating.
------------------------------------------

I might just continue dissolving flakes/powder into it, until its saturated. Any idea what the maximum g/L is?

Edit - nevermind, I found it. http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=37&t=5677


----------



## Barren Realms 007

You can use and old coffee maker base with an element to help evaporate your solution down. Try to use as even of a glass as possible. A thick bottom and thin side can cause the glass to crack because it heats and cools unevenly.

concentration g/l. Hmmmm Well how does 18 Toz/L sound to you. :mrgreen:


----------



## UncleBenBen

Grelko said:


> , I might just order a beaker.



One of the best investments I've made so far. Wish I would have done it sooner. Like Barren said, the thick bottom and thin sides of the Mason jars can't handle the heat, especially if you hit them with a torch flame like I did!



Grelko said:


> I need to work on using less solution next time



That's another thing the beakers helped me with. I got a set of 5 off of Amazon for about 20 bucks delivered. From 50ml up to 1000ml.
Being able to size the beaker to the material, along with the graduated ml marks helped me drastically reduce the amount of acid I used.

Looking good Grelko! Thars gold in that thar spoon!

Ben


----------



## Grelko

Barren Realms 007 said:


> You can use and old coffee maker base with an element to help evaporate your solution down. Try to use as even of a glass as possible. A thick bottom and thin side can cause the glass to crack because it heats and cools unevenly.
> 
> concentration g/l. Hmmmm Well how does 18 Toz/L sound to you. :mrgreen:



I have a "regular" hotplate from Walmart that I've been using, along with a "little" ceramic crock pot insert (maybe 2 L), to evaporate small amounts of used solutions, so that it doesn't bother my neighbors too much. I was thinking about putting the solution into that, evaporating it and transferring it back into whatever I'm going to use to precipitate it in.

I was thinking about leaving the solution in the mason jar, put it in a large crock pot along with some water and see if I could float the jar while evaporating. The water should heat it evenly, but I don't want to chance it breaking, so I won't be doing this.

18 Toz/L sounds great If I had enough material to actually put that much in there. :lol: I might be able to put in about 10g right now, but it'd probably be half of that, since the powder/flakes are dirty.



UncleBenBen said:


> One of the best investments I've made so far. Wish I would have done it sooner. Like Barren said, the thick bottom and thin sides of the Mason jars can't handle the heat, especially if you hit them with a torch flame like I did!
> 
> Being able to size the beaker to the material, along with the graduated ml marks helped me drastically reduce the amount of acid I used.



I'll probably just end up ordering something off of Amazon. Having actual beakers etc, to do this properly, will make things easier.

The markings on the side should be alot better than what I'm using right now. The mason jar markings are too spread out "200, 400"


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## richard2013

Question folks will evaporation with use of hotplate not cause lost of value?


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## jason_recliner

> I was thinking about leaving the solution in the mason jar, put it in a large crock pot along with some water and see if I could float the jar while evaporating. The water should heat it evenly, but I don't want to chance it breaking, so I won't be doing this.


You are certainly an ideas man. But I foresee your boat capsizing. Also the high humidity over your jar from the hot crock water will reduce the rate your solution evaporates.
Best to stick to the tried and true, standard methods:
- Cleanest straightest vessel possible for precipitating.
- Widest vessel possible for evaporating on gentle, dry heat (not in a steam bath). Sand layer for hot hotplates, but they should not be too hot; it should be slow and gentle. A catch dish is extra safe in case of cracks.



> Having actual beakers etc, to do this properly, will make things easier.
> 
> The markings on the side should be alot better than what I'm using right now. The mason jar markings are too spread out "200, 400"


Beakers are a lot better. You will never look back. But the graduations are a guide so don't rely on them.


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## Grelko

richard2013 said:


> Question folks will evaporation with use of hotplate not cause lost of value?



I wondered about this also. What are the chances that the fumes coming from the solution contain gold chloride? Or is it heavy enough that it won't leave in steam form? As long as you don't boil it, you shouldn't need to worry about too much splashing out.



jason_recliner said:


> I was thinking about leaving the solution in the mason jar, put it in a large crock pot along with some water and see if I could float the jar while evaporating. The water should heat it evenly, but I don't want to chance it breaking, so I won't be doing this.
> 
> 
> 
> You are certainly an ideas man. But I foresee your boat capsizing. Also the high humidity over your jar from the hot crock water will reduce the rate your solution evaporates.
Click to expand...


I thought about this also but didn't post it.

I could attach a dowel rod, a couple feet above the crock pot, with 3 strings tied around the top of the mason jar in a triangle pattern, basically hanging the jar in the water, to prevent it from falling over. (It depends on the string because some types may dissolve from the fumes)

The high humidity problem might be countered by placing a fan near it, to blow the steam/fumes away from the top (unless you did want it to evaporate slower for some reason.) 

[stt]The fan would need to be higher than the crock/jar and facing slightly downwards, so that it'll blow air on to the far side of the jar also, or you would still have humidity built up from the lack of air flow on that side.[/stt] (Forget this 1, the current of air from the fan would flow at an angle into the jar, possibly creating a small vortex of condensation droplets, that would roll back into the solution as the steam was being cooled by the fan, negating at least some of the evaporation in the process)[ :lol: partially self distilling solution?]
--------------------



jason_recliner said:


> Best to stick to the tried and true, standard methods:
> - Cleanest straightest vessel possible for precipitating.
> - Widest vessel possible for evaporating on gentle, dry heat (not in a steam bath). Sand layer for hot hotplates, but they should not be too hot; it should be slow and gentle. A catch dish is extra safe in case of cracks.



I'll just stick with this method. It will definately be alot easier, than trying to rig something up and having it break unexpectedly.



jason_recliner said:


> Beakers are a lot better. You will never look back. But the graduations are a guide so don't rely on them.



I'll see if I can find some decent ones on Amazon etc. I should be using better glassware than a mason jar to do this anyways.


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## jason_recliner

> I could attach a dowel rod, a couple feet above the crock pot, with 3 strings tied around the top of the mason jar in a triangle pattern, basically hanging the jar in the water, to prevent it from falling over. (It depends on the string because some types may dissolve from the fumes)


I didn't see where the hamster fits into this recipe for disaster.
No! Just no! Stop this madness now!

Use a hotplate, a coffee maker, or a camp stove and a corning dish, or some other safe, stable and even heat source. It's not that difficult.

Gold will not evaporate at the 80-90 C or so you should be doing this. If you see any bubbles, then turn it down because it's too hot.


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## Grelko

jason_recliner said:


> I could attach a dowel rod, a couple feet above the crock pot, with 3 strings tied around the top of the mason jar in a triangle pattern, basically hanging the jar in the water, to prevent it from falling over. (It depends on the string because some types may dissolve from the fumes)
> 
> 
> 
> I didn't see where the hamster fits into this recipe for disaster.
> No! Just no! Stop this madness now!
> 
> Use a hotplate, a coffee maker, or a camp stove and a corning dish, or some other safe, stable and even heat source. It's not that difficult.
> 
> Gold will not evaporate at the 80-90 C or so you should be doing this. If you see any bubbles, then turn it down because it's too hot.
Click to expand...


Please don't be offended. I was just responding to "the boat capsizing". I wasn't actually going to do this, it was just another idea. *DON'T try this. It would be VERY UNSAFE.*

I posted at the bottom, that I was going to use the "tried and true, standard method" instead of trying to make something that might break.

I am going to transfer the solution from the mason jar, into a crock pot and slowly evaporate it on a hotplate. (The same way I evaporate my other solutions). I don't want to chance breaking the glass.

I should have re-worded my question about the gold chloride. I know it wouldn't evaporate at that temperature. I should have instead asked, if the particles in solution were light enough to be carried off with the steam.


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## Barren Realms 007

You can test to see if you are loosing values while evaporating by putting a coffee filter or paper towel over the opening then one it has moisture on it remove it and test it with stannous.


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## UncleBenBen

jason_recliner said:


> I didn't see where the hamster fits into this recipe



Ha-ha! Isn't it obvious? The hamster is running on that wheel that turns the gears in Grelko's head.
Apparently that furry little guy never stops running, because Grelko's gears are always churning!

Got to admire that!!


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## upcyclist

Grelko said:


> I have a "regular" hotplate from Walmart that I've been using, along with a "little" ceramic crock pot insert (maybe 2 L), to evaporate small amounts of used solutions, so that it doesn't bother my neighbors too much. I was thinking about putting the solution into that, evaporating it and transferring it back into whatever I'm going to use to precipitate it in.
> 
> 
> UncleBenBen said:
> 
> 
> 
> One of the best investments I've made so far. Wish I would have done it sooner. Like Barren said, the thick bottom and thin sides of the Mason jars can't handle the heat, especially if you hit them with a torch flame like I did!
> 
> Being able to size the beaker to the material, along with the graduated ml marks helped me drastically reduce the amount of acid I used.
> 
> 
> 
> I'll probably just end up ordering something off of Amazon. Having actual beakers etc, to do this properly, will make things easier.
Click to expand...

You may have already talked through the evaporating enough to figure out how you'll proceed, but keep in mind that you have a chance of losing values every time you transfer your working material from one container to another. It's like when I work with new[er than me] silversmiths. I tell them to save every little silver filing. Not because silver is that valuable, but because they'll have good habits when they start working with gold. It's the same for us, even though neither you nor I are up to ounces per liter concentrations.

I collected a bunch of wide-mouth Mason jars before I learned the hard way that they don't get along with hotplates, even in baths. Luckily, I had been using ceramic tumbler pellets instead of sand, and had precipitate (fine particles), so it was relatively easy to rinse down the pellets in a sieve, spoonful by spoonful. I'm sure I still lost a lot of values, though. Lordy, rambling again.

Anyway, the mason jars are good for some things, just not reacting in heat. They'll still work for storage and room-temperature dissolution (if you have the time to wait for it), but use the wide-mouth jars if you can, because they have the straight sides you need. You can also get the plastic lids for 'em, so you won't have to worry about the metal corroding in the acid vapors.

All that being said, beakers are better


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## Grelko

Barren Realms 007 said:


> You can test to see if you are loosing values while evaporating by putting a coffee filter or paper towel over the opening then one it has moisture on it remove it and test it with stannous.



Thank you, I will remember to do this while I'm evaporating.



UncleBenBen said:


> jason_recliner said:
> 
> 
> 
> I didn't see where the hamster fits into this recipe
> 
> 
> 
> 
> Ha-ha! Isn't it obvious? The hamster is running on that wheel that turns the gears in Grelko's head.
> Apparently that furry little guy never stops running, because Grelko's gears are always churning!
> 
> Got to admire that!!
Click to expand...


The gears in my head are powered by a self sustaining Aeolipile not a wheel. :lol: The hamster is more of a squirrel though. I think every once in a while, the squirrel gets caught in one of the gears and it gets flung against the wall, which could explain the migraines I get.

*I am always full of ideas for everything, but some of them might not be safe. So if you happen to see me posting a strange way to do certain things, please do not try them.*



upcyclist said:


> You may have already talked through the evaporating enough to figure out how you'll proceed, but keep in mind that you have a chance of losing values every time you transfer your working material from one container to another.
> 
> Anyway, the mason jars are good for some things, just not reacting in heat. They'll still work for storage and room-temperature dissolution (if you have the time to wait for it), but use the wide-mouth jars if you can, because they have the straight sides you need. You can also get the plastic lids for 'em, so you won't have to worry about the metal corroding in the acid vapors.
> 
> All that being said, beakers are better



That's why I should use beakers. Instead of always needing to transfer from a mason jar, to the crock pot, back and forth to see if I need to evaporate more, which is just more of a chance to lose material. (Or just transferring solutions which add to the waste from rinsing it out with water each time.)

I'll have to look around for the wide mouth, straight sided jars to keep certain solutions in. I have a few with plastic lids, but they're being used right now. I have some with the metal lids (the lids are rusty from HCl vapors), so I need to get new ones instead of having pieces of the lid fall into the solution.

I'm slowly getting the proper materials and glassware I need to do these processes. Next on the list is going to be a set of beakers.


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## Barren Realms 007

Once you start using the proper glassware you will never go back to the old stuff.


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## upcyclist

Barren Realms 007 said:


> Once you start using the proper glassware you will never go back to the old stuff.


Agreed! It's all about figuring out what works in the meantime and prioritizing. I ordered some more good glassware from Jade when I purchased some nitric from them, but am still using coffee filters and a plastic funnel--a Büchner funnel and some vacuum power is still on my wishlist. I have a small (5cm) funnel and proper filter paper for testing and small runs, but nothing big for production.

On the Mason jars, btw, the pints are completely straight-sided, the quarts have a small shoulder (but certainly not as bad as a regular mouth quart). My girlfriend, her mom, and my mom all do a lot of canning, so those were freebies. I have a box of 'em that only come out of the box as I use them, so I know which ones can actually return to canning service as I accumulate the proper lab glassware.


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## Grelko

Barren Realms 007 said:


> Once you start using the proper glassware you will never go back to the old stuff.



They finally got here. :mrgreen: 

Lab tongs, 3 glass stir rods, and a 5 piece beaker set. "50, 100, 250, 500, 1000mls" (Beakers are borosilicate)

This will be ALOT better and safer, than using a turkey baster and mason jars. The only thing is, is that I'm left handed, so all of the markings for mls are on the wrong side of the glass. :lol: Also, I bought a few pipettes the other day.


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## Barren Realms 007

Karter!! Who makes carter? 

Markings are on the wrong side. :lol: . You will learn to to be holding your labware when you are pouring solutions in them. 8) 

Tongs!! Never had any and don't have a need for them. Just a nice heavy set of gloves.  

I get tired of breaking stir rods too.


Your getting there. You will like the new stuff. It is a lot better to work with. Congradulations. 8)


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## Smack

Think about getting rubber tips for your stir rods or just tape them so you use the same end to stir with every time. Won't be long before you'll want a couple more 1000ml or 1500ml beakers.


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## jason_recliner

My good sir, your markings are only a guide anyway to let you know how full it is. And the bonus of the beakers being glass is that you can see your markings from the other side! As Barren alluded, when pouring into a beaker if you tilt the receiving beaker you never have a splash. Just like pouring a beer.

Congratulations on getting some decent glassware. You'll only ever want more from here so you'll start dedicating them to tasks. While they're clean and new, choose now one for precipitation; use it for nothing else. It will help your drop and your purity.

Those white areas are also perfect (possibly made?) for marking the tare mass of the beaker. That's really useful when you don't want to move powder just to zero your scales.

Finally, I can't help but nit-pick a constant usage that makes me cringe. A lot is two words that mean a batch, a number, many or much. Allot is to assign or allocate. Alot is not a word. Stop destroying English!


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## Grelko

Barren Realms 007 said:


> Karter!! Who makes carter?
> 
> Markings are on the wrong side. :lol: . You will learn to to be holding your labware when you are pouring solutions in them. 8)
> 
> Tongs!! Never had any and don't have a need for them. Just a nice heavy set of gloves.
> 
> I get tired of breaking stir rods too.
> 
> 
> Your getting there. You will like the new stuff. It is a lot better to work with. Congradulations. 8)



https://www.kartersci.com , but I got mine off Amazon.

:lol: I have to do the same thing with a measuring cup when cooking. I just fill it up with the markings correct, but turn it around to pour. I can always put marks on the other side if I need to.

I figured I'd see how the tongs and stir rods worked. Those long plastic white spoons work pretty good, but I do need to get another good pair of gloves one of these days.

This would work alot better if I actually had the room for a proper lab setup. I just get to work out behind the garage for now.



Smack said:


> Think about getting rubber tips for your stir rods or just tape them so you use the same end to stir with every time. Won't be long before you'll want a couple more 1000ml or 1500ml beakers.



I'll probably use electrical tape for now.

Once I finally get around to working on my material more often, I'll be getting all sorts of things.



jason_recliner said:


> My good sir, your markings are only a guide anyway to let you know how full it is. And the bonus of the beakers being glass is that you can see your markings from the other side! As Barren alluded, when pouring into a beaker if you tilt the receiving beaker you never have a splash. Just like pouring a beer.
> 
> Congratulations on getting some decent glassware. You'll only ever want more from here so you'll start dedicating them to tasks. While they're clean and new, choose now one for precipitation; use it for nothing else. It will help your drop and your purity.
> 
> Those white areas are also perfect (possibly made?) for marking the tare mass of the beaker. That's really useful when you don't want to move powder just to zero your scales.
> 
> Finally, I can't help but nit-pick a constant usage that makes me cringe. A lot is two words that mean a batch, a number, many or much. Allot is to assign or allocate. Alot is not a word. Stop destroying English!



That's why I made sure and got the glass ones 8) I normally pour liquids like that, especially a can of soda, so It keeps more of the carbonation.

I was probably going to use the 250 first, it'll be used for the solution on the other page. I just need to evaporate most of it first. (I also need to read about cleaning them again)

That seems likely, since that's what I was going to use them for. I need to get a new scale :| I banged it on the side of the table and the glass plate you set items on, came off. It didn't break, but it won't sit level anymore.

I still seem to do that with certain words. If you noticed in some of my other posts, I kept having to fix the spelling of the word "separate". I kept spelling it as seperate.


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## butcher

Those of us who live in different parts of America have done a great job of destroying the English language. Or influencing it.
The English language has changed over the many centuries, with many different peoples dialects, and culture or even former languages influencing or even changing the words or spelling it looks like we are not the only ones destroying the language.

https://en.wikipedia.org/wiki/History_of_English


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## Grelko

butcher said:


> Those of us who live in different parts of America have done a great job of destroying the English language. Or influencing it.
> The English language has changed over the many centuries, with many different peoples dialects, and culture or even former languages influencing or even changing the words or spelling it looks like we are not the only ones destroying the language.
> 
> https://en.wikipedia.org/wiki/History_of_English



It has definately changed very much over the years. I still use the term "yinz" and say the word creek as "crick" :lol: There are already so many slang terms/pronunciations, and new ones come out frequently. Just the "slang terms" used for the word dollar or money, is an extremely long list.


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