# First batch good bad really dumb??



## GaryR (Mar 22, 2022)

First batch good bad really dumb??

Hello from Ohio,
I have been following this forum and youtube videos for some time now
and thought it was time to take the plunge...I think i am drowning.
How far am i off here and where to go from here? Please be kind
Decided to just to 10kt for the initial run.
figured out to 63.56 grams gold 41% and 177.94 grams .925 silver
Used too short of a bucket for the inquarting and ended up with some cornflakes 
and some globs. put it all in the flask.
Only had a 1000ml flask so I used about 450ml lab grade hcl on medium heat
and added about 3ml at a time lab grade nitric until each reaction simmered,
getting up to about 40ml nitric when i got a little anxious and it boiled over on me. 
I quit at that time and let it all cool.
filtered off the solution. Filtered solution was kind of yellow, not real
pretty like sreetips batches.
I sprinkled smb in there and it all turned coal black and layers kind of danced/rolled around
in the solution. I let it settle overnight and it is this green color...Sprinkled a 
little more smb until it quit reacting. Looks like a little gold/brown powder dropped out.
Green color is copper i think...10kt has a lot of copper i believe.
Question is the aqua regia still useable after using smb? 


Ended up with some sludge and chunks in the filter. I do not have a vacuum filter so I did not 
rinse this initial batch. 
What to do now with the sludge? dry it, burn the filter and do another batch??
There are 2 ounces of gold in here somewhere by my calculations.


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## FrugalRefiner (Mar 22, 2022)

No.

Before I expand on my answer to your first question, what did a stannous chloride test show before and after you added the SMB?

Now, to your question of whether the aqua regia is still useable after SMB, no.

Next, get yourself some proper beakers. You're lucky your carafe didn't break. It's not meant for this. Borosilicate glass beakers are.

When you boiled over, did you have your carafe in a secondary container to catch the boil over? Buy a pyroceram (like Corning Ware) dish large enough to hold the contents of your primary vessel (beaker) so if it boils over or fails, you'll capture your solution.

Since you have a lot of undissolved sludge, I'm going to guess that much if not most of your gold is there. Scrape it into a beaker, rinsing as much of the sludge off the filter as possible with a minimum amount of water. Then create new AR to dissolve the sludge. Save the filter for later processing when you have a bunch of them.

Dave


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## GaryR (Mar 22, 2022)

Thanks for your reply.
I do not have any stannous chloride so i am winging it.
The Carafe was only used with the smb. I have an actual flask that 
I used with a catch basin. Stainless steel but still a catch.
The green fluid remaining. Am I correct that it is likely copper
thanks gary


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## Martijn (Mar 22, 2022)

The remaining solution will be most likely copper, yes. 
To test for pm's in solution without stannous: put a piece of clean shining copper wire in the solution. If it turns black, there will be pm's in solution. 
To make stannous chloride: dissolve a gram or two in 10 to 20 ml of HCl. 

Did you start with 63.5 grams of 10K or 152 grams of 10K? 
Because 63.5 grams of 10K is about 26.5 grams of gold and 79.5 grams of silver or base metals are needed in the alloy in total to bring it to 6K. 
63.5 minus 26.5 is 37 grams of silver or base metals allready in alloy, so adding 42.5 grams of silver (pure or sterling) would have been enough for inquarting. Saving on roughly 150 ml of nitric. 

Anyway....

Here's where i think you went wrong:

To avoid the creation of AgCl, inquarted gold is treated with distilled water and nitric. No HCl. 
The silver and base metals dissolve in nitric and the gold is left untouched to refine further.

Did you really go for AR with 2.6 Karat gold? (11% gold alloy in stead of 25%) 

You say you quit half-way without digesting all the metal and probably only have a fraction of the gold in solution. The most of your gold, if not all, will still be in your undissolved metal. I AssUMe. 

Silver alloy in AR is covered with a layer of AgCl which stops the digestion of the alloy. 

Judging your questions and actions, you have to slow down and study first. And get some proper equipment. 

Martijn.


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## GaryR (Mar 22, 2022)

OK Let me back up here...
Not having a steamer I boiled it all stirring it in distilled water and a drop of dish soap and rinsed it after removing anything not gold. Then I charred each piece with a cutting torch to burn off anything not wanted. I have read that this procedure dislikes contaminents.

I started with 63.5 grams of pure gold and 177 grams of 925 silver. I figured it to be 20 some percent. With 10kt and sterling there would be a lot of copper.
inquarted it into too short of a bucket and ended up with some oversize nuggets along with some nice flakes. I figured the bigger globs may not digest.
I used a heated nitric /distilled water solution to put the silver into solution (I do not know the exact terminology) then I decanted the solution after it cooled. Rinsed it a few times with distilled water adding the rinse water to the solution.
I then dropped the silver with uniodized salt. Halfway through I looked at the salt ingredients and there is a yellow something in with the salt. Hope it did not hurt? Anyway there is a large batch of white gunk /silver, maybe 1 inch thick in a commercial glass coffee pot. So I figure i have recovered most of the silver.

With the ar I did quit part way and did not digest it all ...not even close. And I did use a Laboratory flask but only 1000ml
Question: is there a calculation for the quantity of HCL needed to digest a given quantity of metal? I think I reached a saturation point in this first batch. If i am correct i need a much larger container.
To make stannous chloride: dissolve a gram or two in 10 to 20 ml of HCl. A gram or two of copper?
I know i am not too smart but hopefully i am not too far off the mark here.


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## BlackLabel (Mar 23, 2022)

GaryR said:


> To make stannous chloride: dissolve a gram or two in 10 to 20 ml of HCl. A gram or two of copper?


No, stannous chloride is made from tin (stannum is Latin for tin) dissolved in HCl until saturated.
Don't tighten the lid! The dissolution will go on for a few days and produces hydrogen gas.

Check out this video:


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## Martijn (Mar 23, 2022)

Check out Wikipedia for the elements, acids and compounds or salts you create.
There you can see how soluble a salt is. For Auric Chloride it's 680 g/L. For every mole of gold (197gr.) there is three moles of chlorine 3×36= 108 gr. So about two thirds of AuCl is gold, one third is chlorine by weight.
That comes to 372 grams of gold per liter water solubility. In HCL it may be higher.
When warm it's also higher. 
When a solution is saturated, crystals are pushed out.
Check out MSDS of compounds to see which safety precautions are advised.

You need the HCL for the HNO3 to react to dissolve the gold and to provide Chlorine for the Auric Chloride to form.
For each gram of gold you need about 1ml of HNO3 in an abundance of HCL in a ratio 1 to 3
If you are going to disdolve one gram of gold, one ml of HNO3 and three ml HCl is needed. 
For each gram of silver in nitric you need about 1.25 ml 70% in distilled water 50/50 ratio. 
For copper it's about 4ml HNO3 in 50/50 acid water ratio.


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