# Just Finished my FIRST ever GOLD BAR 1.025 Troy Ounce



## kadriver (Nov 8, 2010)

I am exhausted. I worked all last night and most of this evening to get my first gold bar. Amazingly it weighs just over 1 troy ounce (1.025 ozt). I could'nt believe it when I put it on my scale (I said a prayer before I melted and poured).

I became interested in refining a little less than a month ago. I assembled a considerable refining lab in the garage of a vacant property we own.

I used 49 grams of karat 14k gold with a touch of 18k and 10k.

I sell scrap gold, and get a good price for it.

I was scared to death that I was going to mess this up and destroy the gold somehow.

Tonight I am my wife's hero (this bar will pay for my lab). I am also a very satisfied and thankful new refiner - you never forget the first one.

Thanks for looking.


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## skeeter629 (Nov 8, 2010)

Awesome job! You should be very proud.


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## joem (Nov 8, 2010)

Great job.


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## Anonymous (Nov 8, 2010)

kadriver said:


> you never forget the first one.


Wanna bet? You didn't see how small my first one was.
Congrats,that is some beautiful gold bud.


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## HAuCl4 (Nov 9, 2010)

8)


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## butcher (Nov 9, 2010)

nothing like the wieght of that shinning yellow metal in a pretty ladies hand to make her accept your new hobbie, great job.


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## lazersteve (Nov 9, 2010)

Excellent bar with nice color! Great job.

Remember that there is always room for improvement.

Steve


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## kadriver (Nov 9, 2010)

Here is a better picture of the bar


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## Barren Realms 007 (Nov 9, 2010)

That color is very nice. 8)


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## Dave English (Nov 9, 2010)

That's beautiful. The large photo is going to give me gold fevor all over again! Great job.


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## Harold_V (Nov 10, 2010)

kadriver said:


> Here is a better picture of the bar


Very nice, and I hope you don't mind some constructive discussion. Please understand that I am not trying to diminish your accomplishment, but to enhance your future results. 

Note the surface of the bar----where it has a rose color, but not consistently. Sort of a coarse speckled covering. That's oxidized base metals of some description. Your gold needed further attention, depending on your objective. It most likely is not up to industry standard of 9995. 

When you melt gold, if it's pure, it remains clear and shiny. When it's contaminated, notice that there's a film on the molten gold that constantly moves from the center of the molten mass to the edges. That's the base metal oxides being absorbed by the flux at the edge of the molten mass. You can cover the mass with flux, which will eliminate the coating, but it doesn't eliminate the contamination. You can also sprinkle a covering of borax on a button the moment it solidifies, which will also remove the oxide coating, but it won't improve the quality of the gold. If it is re-melted, the oxide still exists. 

I found, through the years, that eliminating the condition we're discussing was quite difficult with a single refining, even when good and proper washing procedures were employed. I finally succumbed to refining a second time, which improved the quality immeasurably. 

Having said my piece, if your purpose is to recover and sell to a buyer that resells to a refiner, it likely makes no difference, but if you end up with the opportunity to sell to a consumer, your quality should be such that it does not yield problems for him/her. Not only does that create trust, but it also can lead to a customer in need of refining. 

Nice job, overall!

Harold


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## Oz (Nov 10, 2010)

I will add one thing to what Harold said. If you are selling to an end consumer as having fine gold it goes without saying that it must be .9995 fine. If it is a jeweler that is making up alloy for casting a new piece of jewelry, the number 1 thing you need to have removed from Karat gold scrap (other scrap as well) is lead. The jeweler can deal with most contaminates found in karat gold refining other than lead used in poor repairs or gold fill. The lead is very injurious to the gold as to workability. 

If you are honest with a jeweler as to your gold product he may well work with you on purity as long as you keep the lead out with a touch of sulfuric before precipitation.


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## kadriver (Nov 10, 2010)

I may take Harolds input and re-refine the bar. 

In Hoke, there is a proceedure that removes lead.

It seemed rather lengthy, but appears worth it.

Hoke says to add sulfuric acid to the aqua regia and boil it down to syrup.

Then add hydrochloric. It says that this removes excess nitric acid

Plus it removes LEAD.

I will study this process some more and get everything strait.

Then I'll set up to refine the bar again to the proper purity.

Thank you for your help.

I welcome all criticism. I am very interested in getting it right on.

kadriver


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## norcalmatt (Nov 10, 2010)

kadriver,
Thanks for the very informative and picture heavy posts. I am a little ways behind you and would like to say that
I really appreciate the posts you have started. I am new to this also and "Getting it RIGHT" is the best way and criticism
from these guys will only make the final product better. I look forward to reading more from you and hope to contribute a bit
as well. Keep those posts coming.
Matt


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## Harold_V (Nov 11, 2010)

kadriver said:


> In Hoke, there is a proceedure that removes lead.
> 
> It seemed rather lengthy, but appears worth it.


Actually, the procedure is lengthy because of the nitric, not because of any lead that may be present. For those that evaporate instead of using urea, the only difference in time is the few seconds it takes to introduce a few drops of sulfuric to the solution. The addition of sulfuric causes any lead that may be present to precipitate as lead sulfate, which is then removed in filtration, prior to precipitation. 

As Oz suggested, gold can be "contaminated" with various elements with relatively low harm (although that's not desirable), but even traces of lead destroy its ductility. It is said that molten gold can absorb fumes from lead being melted in the same environment. They have a strong affinity for one another. For the bench man, that spells death, for they can't set stones in gold so contaminated without breaking the prongs or burrs. 

Regardless of the source of the gold I processed, every lot received a few drops of sulfuric, as insurance against lead that may have inadvertently slipped in to the process. You just never know. 

Harold


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## kadriver (Nov 11, 2010)

Please, let me make sure I have this right:

Once the gold is dissolved in aqua regia, then I add a few drops of sulfuric acid to the solution.

The sulfuric acid will precipitate any lead in the solution as lead sulfate which is filtered out at the first filtering.

Then proceed as before with the rest of the process....

This seems too easy to be true - but I will do it when I process the gold bar.

I actually read Hoke AFTER I had gottne to the sodium metabisulfite stage with the gold bar.

I did not roll the gold into thin sheet and then cut into small pieces.

I did not anneal the pieces first.

I did not treat with nitric acid.

On this next refinement I will make sure to include these pre-treatments, and make sure and add the sulfuric acid once the gold is dissolved in AR.

One question - is it true that lead sulfate will dissolve in hot water? If this is true, and one is not carefull, then it seems possible that the lead could end up back in the AR-Gold solution - does this sound correct?

Please give me all the criticism you can pile on - that is why I am here!

Thank you - kadrive


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## Harold_V (Nov 12, 2010)

kadriver said:


> Please, let me make sure I have this right:
> 
> Once the gold is dissolved in aqua regia, then I add a few drops of sulfuric acid to the solution.
> 
> ...


Correct. However, considering you're processing karat gold, my recommendation is for you to inquart. It's one of the ways you can eliminate a huge amount of base metal, thus yielding somewhat cleaner gold. 



> I did not roll the gold into thin sheet and then cut into small pieces.
> 
> I did not anneal the pieces first.
> 
> ...


Make it easy and just melt when inquarting, stir well with a graphite rod, then pour the inquarted material in a deep metallic vessel filled with water. You'll end up with what I like to call "corn flakes", which readily dissolve in dilute nitric. (When poured over the lip of a melting dish, you don't get shot.) Do not pour to a plastic container. It's not uncommon for the molten metal to form a steam cavity and hit the bottom still red hot. Need I say more?



> One question - is it true that lead sulfate will dissolve in hot water?



No. Lead sulfate can be considered insoluble in water, hot or cold. It's lead NITRATE that is soluble in hot water. 



> Please give me all the criticism you can pile on - that is why I am here!


Not necessary. Wise people listen and appreciate helpful tips. You appear to be one of them. 

While the "big boys" tend to process without inquartation, it can be the source of considerable frustration, particularly when you have the misfortune to experience an alloy that is abundant in silver. When the silver content is too high, the material often can't be dissolved in either nitric, or AR. Because the gold content is high, it protects the base metal from dissolution with nitric, and, again, because silver is high, the resulting silver chloride that forms when you attempt dissolution with AR, becomes a hard crust on the surface, isolating the metal from the acid. 

Good luck with your next batch. I expect you'll do a great job.

Harold


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## HAuCl4 (Nov 12, 2010)

What irks you the most Harold?. Silver chloride or lead sulphate?. :lol:


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## kadriver (Nov 12, 2010)

I will do the inquartation with this bar as well and pout into a METAL container filled with water.

I remember reading about inquartation in Hoke which says to use silver, clean copper, or clean brass.

I have some clean silver.

Is silver the best metal to use for the inquartation since I can recover it later? 

Thank you again for all the input.

kadriver


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## HAuCl4 (Nov 12, 2010)

Silver is the recommended metal for inquartation because it requires the least amount of nitric acid and as you said, you can recover the metal later. If you are very careful and thorough and use the 3-1 ratio or more silver to gold, and at the end you boil the gold "mud" that is left in concentrated nitric acid for 15 minutes, and wash thoroughly afterwards, you can produce very fine gold 998-999+. In fact many people do just that and fluxing after.

Here's a great thread to read thoroughly from beginning to end:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=50&t=1275&start=20&hilit=4metals+manganese+dioxide


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## lazersteve (Nov 12, 2010)

There is a video on my website showing gold being inquarted and cornflaked.

Steve


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## kadriver (Nov 12, 2010)

Ok - I think I understand:

Careful inquartation of 3 silver to 1 gold.

Can I use my accet/oxy torch flame to stir the metals?

Then pour molten metal mixture into metal container of water to produce flakes.

Then dissolve the flakes in Nitric acid - leaving a mud which is the gold.

Then, boil the resulting mud in Nitric Acid for 15 minutes.

Then dissolve the mud in AR.

Then add sulfuric acid to precipitate lead sufate.

Then filter and drop the gold.

I know this is simplified, but is this the basic proceedure?

Also: Can I used Liquid Fire available from Ace Hardware for sulfuric acid to precipitate the lead once the gold mud is dissolved in AR?


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## Harold_V (Nov 13, 2010)

kadriver said:


> I will do the inquartation with this bar as well and pout into a METAL container filled with water.


*Don't inquart that bar!* No need. It will dissolve perfectly well in AR now, and that's all that is necessary. Melt the bar, pour the molten gold in deep water (don't use a plastic container) and then dissolve the resulting "corn flakes". Use a clean dish, not one that has melted alloyed gold previously. 

In the future, don't melt your gold if you intend to re-process. Gold powder dissolves quickly in AR--much faster than melted gold. 



> I remember reading about inquartation in Hoke which says to use silver, clean copper, or clean brass.


I always recommend you use silver, and always recommend AGAINST using brass. The problem with copper alloys is you never know when the one you use may contain lead (common in copper alloys, for free machining), but worst of all, you may have aluminum bronze, which yields serious problems for the refiner. Use silver for inquartation ----which consumes far less nitric, and often serves double duty. If you have scrap silver, the typical first step in refining is to part with nitric, so using it for inquartation serves two purposes. 

Harold


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## Harold_V (Nov 13, 2010)

HAuCl4 said:


> What irks you the most Harold?. Silver chloride or lead sulphate?. :lol:


Don't know that either of them was ever a problem. As far as silver chloride is concerned, because I re-processed all my waste materials, I used tap water when dissolving my inquarted metals. The small amount of silver chloride that resulted was recovered when my wastes were run in a furnace, and I relied on the silver to act as a collector. (By the way, it worked very well). 

Because I rarely processed e scrap, I rarely saw any lead, although I always used a few drops of sulfuric in my gold chloride solutions to insure that none was inadvertently carried through the operation. You never know when some manages to slip in. 

Harold


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## HAuCl4 (Nov 13, 2010)

In my very limited AR experience, silver chloride was always the most persistent contaminant, with lead being dealt expeditiously as you have described. Silver chloride just persists and persists, needing chilling the solution before filtering, ammonia washes, etc, and it still persists!.


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## nickvc (Nov 13, 2010)

HAuCl4 said:


> In my very limited AR experience, silver chloride was always the most persistent contaminant, with lead being dealt expeditiously as you have described. Silver chloride just persists and persists, needing chilling the solution before filtering, ammonia washes, etc, and it still persists!.


Oh doesn't it just..... :evil:


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## kadriver (Nov 13, 2010)

Harold - too late. I performed the inquartation. It's ok, I needed the experience - it was kind of fun. But I did loose a few grams in the process.

Here is the result of inquartation.

I started with 31.8 grams of gold (the bar that was previously shown above - it is no longer with us).

I added 99.6 grams of 99.0% pure silver that I cemented using heavy gauge clean copper wire.

I did not have a graphite stirring rod to do this experiment.

Instead I mixed in a piece of silver, then a piece of gold alternately until all the metal was molted in the melting dish.

I then poured the molten metal in a tiny stream into the large metal coffee pot I bought from the Thrift Store ($9.99) I bought for this purpose.

The first time was not too good, I could see some of the gold was heavier in some of the shot, and lighter in the other pieces of shot. (by the way, I could not get flakes, I got shot instead).

I repeated this process 4 times before I finally got a uniform color to each piece of the shot.

Is this how it is supposed to look?

Tomorrow I will dissolve the inquarted gold in Nitric acid.

Then save it for recovering the silver.

Then I will boil the gold mud in Nitric for 15 minutes as previously discussed.

I will then dissolve in AR and make sure and add sulfuric acid to the dissolved gold (I am uncertain about how much sulfuric acid to add).

Then, hopefully, I will precipitate with SMB, wash and melt my newly processed bar of fine gold.

Please let me know if this all looks ok. I will check the forum before I do any of this tomorrow (Sunday).

I am having so much fun that it almost feels like I'm doing something wrong.

Thank you for your input.


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## kadriver (Nov 13, 2010)

Reading back over all the posts i see why I got shot instead of flakes.

I sould have poured the molten metal over the edge of the dish rather that the over the spout.

Also, i did not realize that there was a page 2 to this post. I missed some of your inputs - but learned another lesson.

i must review the entire post, there are so many tips and points that it is hard for me to remember them all. I will make notes as I do this.

Again - thank you all for being so helpful. It is still hard for me to believe that a forum like this exists.

kadriver


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## norcalmatt (Nov 13, 2010)

It seems odd that you lost a few grams during the inquartation. I am new to this also, but I am curious how this loss could have occurred. If you are just melting the metals together and then pouring them into water, there must be some fine bb's or something still in the container.
Matt


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## kadriver (Nov 13, 2010)

Matt:

I lost some when I heated the metal too hot with my torch. When I poured the molten metal into the water, loud bangs were heard like I have never heard before. When I looked in the bottom of the container, my heart sunk - some of the metal had turned to powder!

I tried to recover all that I could by wiping the inside of the metal coffee pot I was using as a quench tank with moist paper towel. Then I opened the paper towel with the silver powder facing up and held it over my electric burner to dry the paper towel. Once dried, I flipped the now dried paper over onto the container with the rest of the metal and popped it with my finger. Of course I could not get all the powder.

I also lost some during handling. Some of these shot were tiny, and they rolled everywhere. If I had been more careful I probably would not have lost a milligram. 

Hope this is helpful to you, Thanks,

kadriver


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## Harold_V (Nov 14, 2010)

kadriver said:


> I did not have a graphite stirring rod to do this experiment.


That's a shame, as it would have prevented the re-melting you experienced. Be certain to stir when you inquart---the metals don't willingly form a homogeneous alloy unless you do. 



> Is this how it is supposed to look?


In your circumstance, yes, but when you inquart karat gold, it won't be as pretty. The amount of base metal that is present (which you should account for when calculating the amount of silver needed to achieve the 25% gold content) will generally give cause for the inquarted metal to take on a different color and shine. No big deal---just a heads-up.



> Then I will boil the gold mud in Nitric for 15 minutes as previously discussed.


The time you subject the material to nitric can vary, but it's important that when you arrive at the finish line, that you have eliminated all of the silver. Otherwise there can be core pieces that won't dissolve in AR. 

My personal preference was to NOT break up the resulting gold---which will be honeycombed--retaining the original size and configuration---but now bronze in color. Breaking it up liberates miniscule particles of gold that are easily transferred when you decant the silver nitrate solution. If you have done your work properly, there is no real advantage to breaking them up----so then, if you choose to pursue that method, don't stir -----that abrades the pieces and breaks them down readily. They're very fragile.



> I will then dissolve in AR and make sure and add sulfuric acid to the dissolved gold (I am uncertain about how much sulfuric acid to add).


At this juncture, very little will be needed. Assuming you poured off the silver nitrate while it was hot, any lead that was present will have been discharged with the silver nitrate solution. If you allowed the solution to cool before decanting, if there was lead present, you may have seen it form in the way of a white substance that settled as the solution cooled. 

I recommend you add no more than ten drops of sulfuric. I expect you won't even need that, but it's good insurance. 

Then, hopefully, I will precipitate with SMB, wash and melt my newly processed bar of fine gold.



> Please let me know if this all looks ok. I will check the forum before I do any of this tomorrow (Sunday).
> 
> I am having so much fun that it almost feels like I'm doing something wrong.


I remember those feelings well (although justified in my case. It was illegal to process gold without a federal license when I started refining. Needless to say, I didn't have one). My first few months in the lab were mesmerizing----and I never grew tired of watching gold precipitate. 

A comment about not inquarting already relatively pure gold----if you re-dissolve it without inquartation, you can see the results of your second refining---the removed contaminants will be found in the barren solution, plus any silver chloride that may have been present may have been removed in filtration. 

Good luck! Be sure to show us the new bar----and take note of the improved color!

By the way---I'm at a loss to understand why you got shot. I poured over the lip of melting dishes for years and never managed to. Only by dispensing through an orifice was I successful. That was true with pure gold, as well as inquarted gold. 

Harold


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## kadriver (Nov 14, 2010)

Harold and the rest:

Thanks so much for your help. 

I just orderd a batch of graphite stirring rods and new melt dishes for next time.

I went back through this post and cut and pasted all the input from everyone to a MS word document. I will keep it close by when I process the inquarted gold.

Also Matt: I found some gold beads adhered to the melting dish - they were gold in color, probably about a gram. I was able to recover some of this, but some wouldn't budge. Hope this is helpful to you.

kadriver


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## Lou (Nov 14, 2010)

HAuCl4 said:


> Silver is the recommended metal for inquartation because it requires the least amount of nitric acid and as you said, you can recover the metal later. If you are very careful and thorough and use the 3-1 ratio or more silver to gold, and at the end you boil the gold "mud" that is left in concentrated nitric acid for 15 minutes, and wash thoroughly afterwards, you can produce very fine gold 998-999+. In fact many people do just that and fluxing after.
> 
> Here's a great thread to read thoroughly from beginning to end:
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=50&t=1275&start=20&hilit=4metals+manganese+dioxide




That's really quite a stretch to say you're getting 3N gold that way.


Lou


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## HAuCl4 (Nov 15, 2010)

Not really a stretch. I assayed my stuff (a while ago) with that process at 9985-9993 in several batches using nitre/bone ash fluxing after copper inquarting and nitric parting. Original material being mine dore and or 18k yellow scrap.

4metals claims consistency at 9995 in a procedure in the thread mentioned above inquarting with sterling silver and using certain flux mix, and I tend to believe him, although I haven't tried the procedure yet. Fluxing can be an art too, I guess.


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## Harold_V (Nov 15, 2010)

kadriver said:


> I found some gold beads adhered to the melting dish - they were gold in color, probably about a gram. I was able to recover some of this, but some wouldn't budge. Hope this is helpful to you.


A part of every refiner's kit should be a cone mold and some soda ash. 

When you find the borax in your dish to contain metals, it's dead easy to remove them. You end up with a cleaned melting dish in the process, albeit at the cost of some of the dish's useful life. I'll explain that, below. 

Heat the dish to redness (using a torch), then add some soda ash. Stir when it's molten, adding more as required. The introduced soda ash will dissolve the existing borax covering, usually well darkened by metal oxides. In the process, it will liberate metals, and allow the tiny prills to agglomerate. Encourage them to do so by playing a torch on them, and directing them towards one another. 

When the mass appears to be homogeneous, pour to a cone mold, which will make separating the values from the slag easy. If you are not happy with the condition of the dish, repeat the process. When you are finished, you can expect a clean dish, ready for use in inquartation again. Be aware that soda ash dissolves the dish, too, so you will sacrifice some of the useful life in the cleaning process. Still, that's better than discarding a dish that contains values that you can't retrieve. 

Harold


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## kadriver (Nov 15, 2010)

Harold, to me you seem like a positive refining genious - I know it comes from your considerable time as a refiner.

I will cut and paste this (like I have with almost all of your other posts) and print it out, and add it to my library for use on my melting dishes.

Not to diminish any of the other folks who have provided me with precious insight into refining. I appreciate ALL the input from ALL forum members.

Thank you again - kadriver


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## Lou (Nov 15, 2010)

HAuCl4,

I'm sorry, I didn't see that there was fluxing involved. I thought you meant straight out of an inquart it's 3N.

Lou


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## kadriver (Nov 15, 2010)

Here is the second refining of the gold bar that has now been inquarted with 3 troy ounces of 99.0% pure silver metal.

I started by adding 120 ml nitric acid to the inquarted metal to dissolve the silver.


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## kadriver (Nov 15, 2010)

the 6k gold shot turned black and looked like coffee beans.


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## kadriver (Nov 15, 2010)

The reaction increased when i added some heat.

Please note that the beaker is directly on the hot plate coil:

DON"T DO THIS, IT WAS A BIG MISTAKE.

PLACE A CORNINGWARE DISH ON THE HOT PLATE AND PUT THE BEAKER IN THE CORNINGWARE DISH.

You will see why this is important in a minute.


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## kadriver (Nov 15, 2010)

When the reaction slowed to a crawl, I used a glass stirring rod and carefully crushed the pieces of brown gold left in the nitric acid.

As soon as i did this the reaction picked back up. I kept crushing the gold mud until there was no more reaction.


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## kadriver (Nov 15, 2010)

I removed the beaker from the heat and this is what was left after i let it settle.


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## kadriver (Nov 15, 2010)

Gold mud after pouring off the silver laden nitric.

I saved the acid to recover the three troy ounces of silver that is dissolved in it.


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## kadriver (Nov 15, 2010)

Here I go doing a second boil in concentrate nitric acid to ensure that all the silver and other base metals are dissolved away from the gold.

All looks well and is going OK for now.

Notice the beaker sitting directly on the coils of the hotplate, disaster is about to strike.

I am new to refining. I learned a costly and important lesson about putting the glass beaker directly on the coil - I WILL NEVER DO THIS AGAIN!

Plus, I am ordering a watch glass to cover the beaker during heating.


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## kadriver (Nov 15, 2010)

The boil was going well. It was a rolling boil, then suddenly it popped and hot acid and gold mud shot about 2 foot straight up.

I was inside watching through a closed window (as I do in all my reactions with heat). I unplugged the hot plate immediately then watched helplessly as the beaker continued to spit hot acid and my gold.

Finally the hot plate cooled and the spattering stopped.

If you are new to this like me, then take note of this mishap and learn from my mistake - NEVER PUT A BEAKER DIRECTLY ON A HOT COIL WHEN BOILING ACID AND GOLD!

Enough said about this - lesson learned.


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## kadriver (Nov 15, 2010)

A close-up of the mess this blunder caused me.

So much for my shiny new hot plate....


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## joem (Nov 15, 2010)

so sorry, now get your metal detector out and start searching under your deck


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## kadriver (Nov 15, 2010)

Here is the remainder of the gold mud being dissolved in aqua regia

Note the corningware dish under the beaker


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## kadriver (Nov 15, 2010)

After about 1/2 hour the gold mud began to look like carrot juice


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## kadriver (Nov 15, 2010)

I slowly added urea to the carrot juice until no mre reaction occured.

Then I added 10 drops of sulfuric acid to remove the lead

I diluted with an equal amount of distilled water and the AuCl looked like orange juice.


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## kadriver (Nov 15, 2010)

Filtering the dissolved gold - note the deep yellow color of the liquid


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## kadriver (Nov 15, 2010)

What was left in the filter paper


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## kadriver (Nov 15, 2010)

here comes the fun part - dropping out the gold with sodium metabisulfite.


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## kadriver (Nov 15, 2010)

The gold began to precipitate before I got done pouring in the SMB


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## kadriver (Nov 15, 2010)

Note the dark brown color like hot cocoa


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## kadriver (Nov 15, 2010)

Pure gold powder at the bottom of the beaker


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## kadriver (Nov 15, 2010)

Stannous Chloride test - there is still gold in the solution.

I added more SMB to get the rest of the gold to drop.

I tested again and the test was clean - all the gold had dropped!


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## kadriver (Nov 15, 2010)

This is what the dropped gold looked like in the bottom of the beaker.

I will let it settle overnight.

Tomorrow I will wash, dry and melt the gold bar.

Thanks for looking - kadriver


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## 4metals (Nov 15, 2010)

Nice pictures, are you powering your vacuum with compressed air?


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## norcalmatt (Nov 15, 2010)

Great picture story kadriver. I am sorry to hear about the mishap, but thanks for sharing your mistake. Hopefully you won't be missing too much gold. Any idea's as to why the beaker "exploded". This post will definitely help me with my first refining. Take care.
Matt


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## 4metals (Nov 15, 2010)

Glass cannot take uneven heat! The coil type of hot plate produces different amounts of heat to the beaker bottom, the glass can't take it. The casserole is a good idea. I notice there is also a tray under the stove for spill containment, another good idea.


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## kadriver (Nov 16, 2010)

4metals:
I am using a air conditioning vacuum pump ($79.95 Harbor Freight).

I bought an old air compressor for $35 and removed the compressor.
I then installed the vacuum pump to draw on the tank.

the flask is connected to the tank, and the compressor draws from the tank.

The air tank acts as a vacuum reservior so the pump is not drawing directly on the flask. i can evacuate the air tank, then use that vacuum to draw on the filter flask.


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## norcalmatt (Nov 16, 2010)

kadriver,
Please post how you clean the precipitated gold when you are finished. I sure hope your new button comes out near and ounce.
Matt


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## kadriver (Nov 16, 2010)

matt:

Tomorrow I plan to do this:

Pour off the liquid and wash with hot water.

Boil the powder in Ammonium Hydroxide to get any silver chloride out.
Boil in Hydrochloric acid to finally remove any base metals that got thru.

Then filter washing with about 1000ml boiling water thru the filter over the gold powder.

then put in a dish and dry over low heat.

then melt it and pour it.

kadriver


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## HAuCl4 (Nov 16, 2010)

kadriver said:


> What was left in the filter paper



Was there much in the filter paper?. I can't tell from the photo.

You were lucky that the beaker didn't "crack". Only obvious tip is to heat the acids (nitric for inquart treatment, HCl for AR) *before* adding to the metal. It seems faster that way, and there is less need for continuous strong external heating. Irons has suggested the use of a microwave oven for quickly heating acids. :shock: 

Very nice pictures of "the craft". 8)

In the picture below you have a beaker in the center, gray is fiberglass (or other) insulating wool, and the outer is a PVC or fiberglass/resin container. If the glass cracks it is not a disaster, and it keeps the solution warm like a thermos. :shock:


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## kadriver (Nov 16, 2010)

4metals:

This is an interesting method. i will give it a try.

I normally use a heavy pyrex coffee pot to boil acid.

I used a beaker this time because the amount was small.

I think from now on I will just break out the coffee pot to boil in.

Thank for your input.

kadriver


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## HAuCl4 (Nov 16, 2010)

Another tip: "Letting it settle overnight" at that point, only helps the ever present silver chloride to drop on top of your precipitated gold overnight. If you are going to leave anything "settling overnight" it should be *before* precipitating the gold to get rid of the AgCl. Some people have suggested inside the freezer or in a very cool place to help the dissolved AgCl drop. :shock: 8)

Can you please post a close-up shot of the filter paper with the AgCl and/or lead sulphate?. It's not clear in the photo you posted. :?:


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## kadriver (Nov 16, 2010)

i will post a better picture of the filter paper. There was not much on it.

Letting the dropped gold container settle overnight seems like a mistake according to what you have posted.

Should I stirr the solution up and then pour it off after just then gold settles?

Also, I plan to boil the gold powder in ammonium hydroxide and then boil in hydrochloric acid - washing in between.

i am not going to filter this batch, just pour off and wash with hot water between treatments.

Once that is complete, I will wash thoroughly and dry the powder.

kadriver


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## HAuCl4 (Nov 16, 2010)

At this point I guess I would stir it as you suggest to try to get the fine AgCl in suspension, but it might be already in little lumps on top of the gold. It wouldn't hurt to stir before decanting and washing, I guess.

Another tip: If you are going to do this often, you need some type of "acid trap" in your vacuum line, otherwise the tank and vaccuum pump will not last very long. 8)


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## kadriver (Nov 16, 2010)

Do you think that boiling the settled powder in ammonium hydroxide would get rid of the silver chloride?

As for the vacuum set-up, after a few uses, I mix up a batch of baking soda and suck about 250 ml through the whole system. Then I drain it off from the bottom of the tank which has a drain valve for this purpose.

I thought about putting an inline filter or trap of some sort down low to collect any acid and other liquids that get through.

On the other hand the components were relatively inexpensive and easily replaced if needed.

I keep my eyes peeled for old air compressors for sale. i will get a spare and have it available in the case that my metal vacuum tank fails due to acid.

thank you
kadriver


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## HAuCl4 (Nov 16, 2010)

I think you are doing just fine with your plan and planned washes, etc. Just adding common sense tips here and there that may be useful to you. 8)


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## kadriver (Nov 16, 2010)

Roger that - Thank you

kadriver


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## HAuCl4 (Nov 16, 2010)

kadriver said:


> i am not going to filter this batch, just pour off and wash with hot water between treatments.



I'd save the liquids and let them settle at least for a few days and cement with a copper bar. Just to make sure I don't throw any values out. 8)

Also don't mix the ammonia wash with the acids!.


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## kadriver (Nov 16, 2010)

here is a better picture of the filter paper


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## kadriver (Nov 16, 2010)

Here is the new bar weight, lost alittle but not too bad.


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## kadriver (Nov 16, 2010)

I am really pleased with the second refining.

The bar is much smoother and has no roughness to its surface.

i can see my reflection in the metal.

I think this one is closer to fine gold - 999

Thanks for the guidance from this forum.

kadriver


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## norcalmatt (Nov 16, 2010)

That is a very nice looking gold bar. I am glad you didn't lose too much of your gold. Thanks again for sharing all the pictures and your experience.
Matt


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## goldsilverpro (Nov 16, 2010)

kadriver,

I want to congratulate you on your progress. You've come a long way in a short period of time. I don't think you've been on here for a month. My hat's off to you.

Chris


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## lazersteve (Nov 16, 2010)

I second Chris' sentiments, you are doing great. The color of the bar looks great!

Steve


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## kadriver (Nov 16, 2010)

Thanks guys - your comments are very encouraging.

kadriver


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## Harold_V (Nov 17, 2010)

I would recommend you do any further _secondary_ (re-refining) refining without melting, and especially without inquartation. Traces of silver that may have been included in the first refining will be removed in the second refining, but, most importantly, the barren solution after precipitation will be a good indicator to you of what is being removed in the second refining. By inquarting, you continue to include one of the things you hope to eliminate---traces of silver. I understand your need to experiment---my comments are meant for the future, whereby you already understand the mechanics of inquartation. 

Drag down is generally the problem with contaminants, assuming you have used a selective precipitant. By the time you have dissolved the once precipitated gold, the traces of contaminants that were present are well diluted by the volume of solution, so secondary drag down is vastly reduced. You can expect good quality, even when the first refining is questionable. That, of course, assumes you use a good washing procedure. How one washes recovered gold is just as important as are the other processes. 

I took note of your comments about using a watch glass. Make that a habit, as when you are dissolving, the vigorous vapors that emanate from the solution carry values with them----including silver from the silver nitrate solution. Keeping your vessels capped with a watch glass minimizes potential losses, plus it makes for much easier heating. 

Well done! I see an absence of the bronze color of the original ingot. 

Harold


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## HAuCl4 (Nov 17, 2010)

I had to put my shades on to look at the bar!. Congrats!. 8)


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## HAuCl4 (Nov 17, 2010)

Harold_V said:


> By inquarting, you continue to include one of the things you hope to eliminate---traces of silver. I understand your need to experiment---my comments are meant for the future, whereby you already understand the mechanics of inquartation.



One of those analytical chemistry types told me years ago, that if I really wanted to make really pure gold, the first thing I should do was to inquart and nitric part twice but with pure *nickel*, before doing any processing with AR dissolution. I thought he was nuts, and I knew better. It only made *some* sense recently, but I have never done it. His reasoning was that he wanted an easily removable contaminant as the main contaminant, and not lead, copper, silver, or PGMs. This was long before solvent extraction was more widely known.

What do you guys think?. :?:


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## kadriver (Nov 17, 2010)

Using nickle to inquart - does it alloy with the gold easily? 

does nickle dissolve in nitric acid as easily as silver does?

Can the nickle be recovered as easily as the silver is for reuse?

Is pure nickle easily obtainable?

Sorry, all I have is more questions - but now I am curious.

This sounds like an interesting new experiment.

Thanks - kadriver


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## HAuCl4 (Nov 17, 2010)

I suggest you pass on this for now. If only because nickel has a relatively high melting point. Let's wait for the other guys to comment, since this is not standard procedure anywhere, and nickel is relatively expensive.


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## kadriver (Nov 17, 2010)

Good suggetion - Thanks


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## Oz (Nov 17, 2010)

Nickel is also far more toxic as a salt or in solution than silver is.


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## Harold_V (Nov 18, 2010)

In a nut shell, I think it's total BS. What possible reason could one have to employ nickel? It's expensive, melts at a high temperature, and creates unnecessary work. Sounds a lot like adding a hand full of dirt to the laundry to insure clean clothes. 

It makes no sense re-introducing ANY contaminant, regardless of the ease in which it can be removed, if your objective is pure gold. The second dissolution leaves no reason for inquartation----no reason at all. If you feel the nitric digest serves a purpose, once precipitated gold can be heated (in a casserole) to insure there are no chlorides present, then the gold washed in dilute nitric prior to dissolution the second time. After all, that's the objective----not inquarting--which does nothing more than reverse the first precipitation. 

Even if the gold to be processed has come from an exceedingly dirty solution, nothing more is added by this method. The resulting solution would, likewise, now contain but a trace of the original contamination, so drag-down would be but a miniscule portion of the original, evident by the color of the barren solution. 

Harold


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## HAuCl4 (Nov 18, 2010)

Harold: 

This is my reasoning and how it makes some sense in my head (not an explanation given by the chemist). It may be all wrong but here it is:

Let's say for the sake of argument that one starts with 1 Kg of 997 gold obtained by silver inquarting and parting with nitric. That's 997 grams Au and 3 grams of X (Ag mostly, with Cu, Pb, Pd, others, etc).

Now one adds 3,000 grams of 999.9 Ni, melts and alloys well (I agree a pain because Nickel has a high melting point, but let's continue).

We have an alloy of 4,000 grams, with 997 grams Au, 2999.7 grams of Ni, 0.3 grams of Y (the Nickel contaminants, whatever they are) and 3 grams of X. The non-gold portion of the alloy is 3003 grams of mainly Nickel, let's call this SHT (insert joke here :lol: ).(2999.7 Ni + 0.3 Y + 3 X).

After parting in nitric again (assuming we get to the 997 level exactly again) we are left with 997 grams of gold and 3 grams of SHT, where SHT is made of 99.89% Ni+ 0.1% X + 0.01% Y. So we can see that the silver, lead, copper, etc contamination has been made in the order of 0.33 grams on average, and the Nickel is now the main contaminant. So if we dissolved this in AR now, we would have very little silver chloride, lead compounds, copper, pgms, etc.

Now if we do the process of alloying again, the contaminants would be very low order traces, and we would basically have 997 grams of gold alloyed with 3 grams of the pure Nickel that we are using.

This new alloy of gold and nickel (after parting in nitric again) would be much easier to use to produce UHP gold, because all the "tough" and persistent contaminants have been diluted, and only Nickel is relevant.

One single dissolution in AR at this point (With UHP chemicals, UHP water, clean vessels, etc), and a DBC extraction/ precipitation and we would be looking at a really pure piece of metal at a reasonable cost.

I guess this is all academic discussion, because there is no urgent need to produce gold beyond 9999 purity. 

I welcome all reasoned criticisms to the above "argument/procedure", and its holes which may be plenty. 8)


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## goldsilverpro (Nov 18, 2010)

It's a waste of time discussing it, in my opinion. Totally impractical, for reasons that Harold already mentioned (and I can think of others).


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## rockpicker1 (Jan 16, 2011)

This is not the first, but it came from 3 lbs. of head ore.


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## rockpicker1 (Jan 16, 2011)

These two came from 16 lbs. of head ore.


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## bhartley (Feb 19, 2011)

I don't have any experience melting gold, but from what I know about melting other metals, it looks like your gold is solidifying as soon as it contacts the mold. I think you'd get a prettier ingot if the gold had a chance to properly fill the mold before solidifying. 

Just to satisfy my own curiosity:
How much are you heating the gold after it melts?
How hot do you preheat the mold?
Do you use a ductile cast iron mold or a graphite one?


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## golddie (Feb 20, 2011)

I think Harold said he never used urea in refining and in the forum I am coming across many post that say they are using this thing.
From what I see it kills the free nitric so that there is less in the air.
I would like to know how much of urea is used in proportion to the quantity of the solution
Thanks


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## goldenchild (Feb 20, 2011)

golddie said:


> I think Harold said he never used urea in refining and in the forum I am coming across many post that say they are using this thing.
> From what I see it kills the free nitric so that there is less in the air.
> I would like to know how much of urea is used in proportion to the quantity of the solution
> Thanks



It's personal preference if you want to use urea or not. It's nice if you want to get to dropping the gold quickly without having to denox. Put a few pellets in and stir completly dissolving the pellets. Continue adding until there is no more reaction (fizzing). If your'e good at managing how much oxidizer you put in with your HCL you won't need it though.


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## Barren Realms 007 (Feb 20, 2011)

goldenchild said:


> golddie said:
> 
> 
> > I think Harold said he never used urea in refining and in the forum I am coming across many post that say they are using this thing.
> ...



Just because it stops fizzing dosen't mean you have gotten all of the nitric out. Especialy if you deal in large volumes of solution.


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## goldenchild (Feb 20, 2011)

Barren Realms 007 said:


> Just because it stops fizzing dosen't mean you have gotten all of the nitric out.



Ok. Not out but neutralized.


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## Barren Realms 007 (Feb 20, 2011)

goldenchild said:


> Barren Realms 007 said:
> 
> 
> > Just because it stops fizzing dosen't mean you have gotten all of the nitric out.
> ...



Even then not totaly neutralized at times. I have 100 gals of solution that I am pumping around to day to see what has settled after it was processed and still showed positive for PM's and I have been cementing the solution with copper. And another 80 gals to filter out today to drop the PM's that I ran on heat to get the nitric out.

It just takes patience to accomplish this at times.


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## goldenchild (Feb 20, 2011)

Barren Realms 007 said:


> Even then not totaly neutralized at times. I have 100 gals of solution that I am pumping around to day to see what has settled after it was processed and still showed positive for PM's and I have been cementing the solution with copper. And another 80 gals to filter out today to drop the PM's that I ran on heat to get the nitric out.
> 
> It just takes patience to accomplish this at times.



Yes. Patience is the key with all our processes. When you are cementing out the PM's, effectively you are also denoxing. I hope you recover a brick Barren 8)


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## Barren Realms 007 (Feb 20, 2011)

goldenchild said:


> Barren Realms 007 said:
> 
> 
> > Even then not totaly neutralized at times. I have 100 gals of solution that I am pumping around to day to see what has settled after it was processed and still showed positive for PM's and I have been cementing the solution with copper. And another 80 gals to filter out today to drop the PM's that I ran on heat to get the nitric out.
> ...



Me too, I will still need to reprocess it once recovered.


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## glondor (Mar 19, 2011)

Hey Barrenrealms007, How did you make out with the 180 gallons of cement solution? I would hope you got a few grams from that volume of liquid.


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## Barren Realms 007 (Mar 19, 2011)

glondor said:


> Hey Barrenrealms007, How did you make out with the 180 gallons of cement solution? I would hope you got a few grams from that volume of liquid.



Pulled a little over 2 oz of gold out of solution that had already been dropped and still showing small positive test for PM's mostly Palladium with a small trace of gold still. I've got some copper powder to dry out that I am going to add to the solution soon and get to a gegative test for PM's.


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## 4metals (Mar 19, 2011)

> Pulled a little over 2 oz of gold out of solution



That's not bad. Considering half of the waste was rinse water and a gallon of aqua regia digests 28 ounces of metal on average, you dissolved about 2520 ounces of metal (if the acid was saturated) and lost 2 ounces of gold. That's only 0.079%. 

See it pays to cement with copper.

Good job.


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## Barren Realms 007 (Mar 19, 2011)

4metals said:


> > Pulled a little over 2 oz of gold out of solution
> 
> 
> 
> ...



Yea, and even with cementing it onto copper for days and recovering this. I am still showing positive test for Palladium and slightly postive for Gold. I am going to use some copper powder I have to dry out and I am going to try and cement the rest out with this.


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## glondor (Mar 19, 2011)

I am glad I have saved all my solutions. That is a fantastic recovery from what many would consider waste. Bet that put a smile on your face.


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## trashmaster (Mar 19, 2011)

that will pay the light bill and buy you 2 or 3 new HOT PLATES


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