Just Finished my FIRST ever GOLD BAR 1.025 Troy Ounce

[lazersteve]

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

Steve

 

[kadriver]

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?

 

[Harold_V]

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

 

[Harold_V]

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

 

[HAuCl4]

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!.

 

[nickvc]

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:

 

[kadriver]

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.

 

[kadriver]

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

 

[norcalmatt]

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

 

[kadriver]

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

 

[Harold_V]

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

 

[kadriver]

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

 

[Lou]

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

 

[HAuCl4]

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.

 

[Harold_V]

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

 

[kadriver]

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

 

[Lou]

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

 

[kadriver]

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.

 

[kadriver]

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

 

[kadriver]

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.