stock pot hiding Au with nitric

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steyr223

Well-known member
Joined
Oct 9, 2011
Messages
930
Location
Fullerton ,California. usa
Hey guys hows everyone

I decided to attack my stock pot 2 days ago
I filled a beaker to 800ml ,evaporated to 400ml
Added Hcl to 800ml ,evaporated back to 600ml
And added hcl once more to 800ml

This material i believe has some gold if not a bunch
I did 4lbs of the goldbacked,gold legs ic's and only yeilded
Around 4 grams/lb amd i believe sam or lou said 1/3 of an ounce( math says roughly 24 grams missing) :shock:

And thats just one item

The problem is too much nitric acid and I can't test for gold that's why I'm evaperating down

I did a stannous test and got nothing
I had put a lot of copper in to try and cement ( it just dissolved the copper)

I decided to filter and look for powders at the bottom which I found a lot I was excited and thought it was gold but then realized it could be anything
I took the filter and put it in Hcl/bleach and filtered twice through a Charmin plug of fiberglass
I tested with stannous and it came up slightly positive very light purple along one edge of the drops

Now I have salts that won't go away and plan to do some testing so I will have more information but for now is there anything else I should be doing

Thanks steyr223 rob
 
the salts will go away with the addition of water

hoke says to evaporate down to a syrup. then ad hcl, you can try sulfamic acid to rid the free nitric.
 
thanks necromancer

Yes i tesed the salts they do not dissolve in a cold Hcl
Or cold ammonia but they do dissolve in cold h2o

this would tell me its just table salt correct

I will try what Holkes says

Thanks steyr223 rob
 
Harold always said to incinerate...
You have evaporated several times so maybe incinerate and then try hot HCL, and what's left, HCL + Bleach and see if it tests +.

Just my guess as to what I will do with my stock material. Although no Nitric in the batches.

B.S.
 
Whatsup pantherlikher
Incinerate what the salts ot the black powder that comes out in my filter(i think it is smb amongst many other things)

I have not filtered my entire
bucket but it did not look like any salts on the bottom
When i decant my bucket i see the black rolling cloud trying to escape

The salt comes from when i dissolution the black powdrt
With Hcl/bleach then filter with fiberglass in funnle
When i come bsck to fimd salts in my beaker

Thanks steyr23 rob
 
steyr223 said:
Hey guys hows everyone

I decided to attack my stock pot 2 days ago
I filled a beaker to 800ml ,evaporated to 400ml
Added Hcl to 800ml ,evaporated back to 600ml
And added hcl once more to 800ml

This material i believe has some gold if not a bunch
I did 4lbs of the goldbacked,gold legs ic's and only yeilded
Around 4 grams/lb amd i believe sam or lou said 1/3 of an ounce( math says roughly 24 grams missing) :shock:

And thats just one item

The problem is too much nitric acid and I can't test for gold that's why I'm evaperating down

I did a stannous test and got nothing
I had put a lot of copper in to try and cement ( it just dissolved the copper)

I decided to filter and look for powders at the bottom which I found a lot I was excited and thought it was gold but then realized it could be anything
I took the filter and put it in Hcl/bleach and filtered twice through a Charmin plug of fiberglass
I tested with stannous and it came up slightly positive very light purple along one edge of the drops

Now I have salts that won't go away and plan to do some testing so I will have more information but for now is there anything else I should be doing

Thanks steyr223 rob
Take a small sample and evaporate off the nitric acid the proper way (down to syrupy). 800 ml is way too much, 10 ml had been more than enough. Then test this sample for gold traces. Excess nitric acid can mask the presence of gold in solution.
If it really is barren then the rest of the solution is also barren and you are chasing a ghost. Siphon off any barren liquid without disturbing any sediments on the bottom. (siphon or use wick filter) The barren liquid is discarded.

If your stock pot is eating metal then you haven't treated it right from the beginning. There should always be excess metal in the stock pot to cement the precious metals. Without free metal you are only storing your wastes.

Hoke gives excellent instructions for the stock pot starting on page 143.

I would not recommend incineration of any gold chloride salts. Both silver chloride and gold chloride is volatile and can easily go up in smoke. Butcher have described how to treat scrap containing chloride salt with NaOH to turn it into hydroxides instead to minimize losses when incinerating.

Personally I like to use HCl + H2O2 or straight AR when redissolving gold as it doesn't add any salts to the solution.

Göran
 
You are right Göran...
The stock pot should have copper metal in it to drop any PMs that made it that far. The sediment after having copper might have PMs dropped from solution.
I'm going by what I have from my pot. Metals in metal form and not a chloride salt. He stated he has what looks like salts as well so it needs to be washed out with water, then hot HCL. This should rid any excess copper or other base metal as well as any salts of metals leaving PM in metal form.
Since he has used nitric, I remember Harold always saying to incinerate to remove any oxides?..not sure but... Incinerating leaves the solids at thier metalic form for the next steps.

This part is hard for me to explain but he has always said to incinerate to start again for processing.

B.S.
 
Thank you both
Göran
It us strange how somethings can be right in front
Of us but we dont see it

For almost 3 years i have been evaperating from
A large amount of solution even for testing purposes
Even after reading holkes
Now that you say 10ml is good i am amazed at why i haven't been doing that all along

I need to point out i had said the salts came from putting my powders in solution (Hcl/bleach)
Not in the stock pot

Also i do apologise if this makes a difference
But i did not use Hn03 directly. I used Hcl/potassium nitrate for the chips
I should have stated excess nitre not Hno3 :oops:


Thanks steyr223 rob
 
It doesn't matter if the nitric acid comes from a mixture of potassium nitrate and hydrochloric acid or directly from nitric acid, the result is the same. It will dissolve gold as long as it is acidic and there are nitric ions in solution.

The problem with potassium nitrate is that an over dose of it stays as a salt. Any over dose of nitric acid is easy to evaporate off without leaving salts.
This is especially a problem for people using urea. When the acid is used up there could be a lot of nitrates left in solution (potassium- copper- iron-... nitrates) that doesn't react with the urea. Then you drop the gold with SMB or some other reagent. So far so god, but when adding HCl to clean the gold it reacts with the nitrate salts left and dissolves the gold again.

10 ml sample size is a lot too, you actually don't need more than you use for the test in the end, but it can be good to have some extra if you want to run more than one test.

I didn't say that incineration was bad, just that incineration of chloride salts can give you high losses. In properly treated materials the chloride ions could be washed away before incineration, but you can't wash gold chloride as it is soluble. You have to "fixate" the precious metals first. In the stock pot the gold chloride is turned in metallic form by cementing on metal. If you have silver chloride it can be turned into silver oxide by NaOH treatment.
Incineration does not remove oxides, it turns base metals into oxides as well as most of nitrates, chlorides, sulphates... into oxides.

Göran
 
steyr223 said:
I had put a lot of copper in to try and cement ( it just dissolved the copper)

That's a clear indication that you have a LOT of free nitric - forget get all the evaporate ad HCL etc. (other chems to rid nitric) just keep adding copper until it starts cementing values & then wait for reaction to stop --- That is standard stock pot procedure - cement values - incinerate - treat as dirty values (water - HCL washes - with ammonia wash ONLY if you think you have Ag/Cl)

Kurt
 
Pantherlikher said:
, I remember Harold always saying to incinerate to remove any oxides?...

I am quit sure Harold's advise to incinerate was to convert metal salt/complex into oxides (not remove them) such as stannic tin to tin oxide or copper chloride to copper oxide etc. - the oxides can then be treated & removed with hot HCL wash

Kurt
 
kurtak said:
steyr223 said:
I had put a lot of copper in to try and cement ( it just dissolved the copper)

That's a clear indication that you have a LOT of free nitric - forget get all the evaporate ad HCL etc. (other chems to rid nitric) just keep adding copper until it starts cementing values & then wait for reaction to stop --- That is standard stock pot procedure - cement values - incinerate - treat as dirty values (water - HCL washes - with ammonia wash ONLY if you think you have Ag/Cl)

Kurt

Hey kurt
There's only one problem with that
I am not that rich and over the last couple
Months i dumped a fair amount of copper
Anyways i probaly should make sure there are
Values before wasting more time and money

I was very careless back then i could have washed my values away before they hit the stock pot :lol:
I was hoping i didn't

I read somewhere on this form (maybe butcher)that
Just because you have a copper hungery solution doesn't
Mean it has values
Please correct me if i am wrong
I will follow görans advice and if the solution
Shows Au then i will dump the copper table inthe backyard in it :shock:
Thank steyr223 rob
 
Rob how much solution is in your stockpot?
I was thinking you could use a weighed amount of steel on a specified amount of solution which would cement the copper and any values, doing the math and working carefully you should be able to cement all the values with a little copper from the rest of your stockpot. Not as neat as copper but possible and cheaper but try it on small amounts to see how it works just put all solids back into the stockpot.
 
Like kurtak said just throw in copper. The boiling down and adding is nuts! What if you had a 5 gallon bucket? But you don't have to use copper if you don't have any available. Iron, and zinc will also work. Then it would just be a matter of getting rid of any copper that cements out. In sponge form it would be very easy.

Afterthought: If you are having trouble getting copper then build up your stash. After isolating and filtering the pms use the same iron/zinc from the first cementation to drop the (undesired) metals again. Filter and dry these and you will have a nice sponge for the next time you need to do a non selective drop.
 
Take a cup of solution and put some copper in it till it stops. If there is something cemented out, then continue.

No matter what you have or not, you still have to drop everything out and dispose of the solution.

My first batch that went into the pot got a couple pieces of steel. CD cases. This dropped copper and anything else there. I moved liquid to another pot with more steel and then on to PH adjustement. I kept adding to the first pot untill the steel was all used(dissolved). Now the pot had copper and any PM so I just kept adding spent solution to the pot. When I thought my AP was full, I put alot into the first pot. And in 2 days, there was no copper left on the bottom. That's when I drained the pots and moved the solids. First pot is what I have to process and test soon. Copper from the second pot with steel, went into the first pot to drop future PMs.

This set up seems to work great as copper drops in the second pot and the only thing I keep adding is steel to drop copper.

B.S.
 

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