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IGutYa said:
shyknee said:
Thank for your help on this " that black powder in hcl+clorox does nothing. hot or not "
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i tried first cold, then brought nearly to a boil & held. the end result was a yellowish-green acid that tests Negative for gold with stannous chloride & all the black powder sitting in the bottom.

i have no doubts that AR will be able to take care of it.
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This is a tread from Steve.


I'm going to assume this black (?) material is from a sulfuric stripping cell.

Here's how I would proceed from this point forward.

1. Rinse the entire contents of the filter into a straight walled beaker and cover the black sediment with HCl to twice it's thickness in depth.

2. Heat to 60C.

3. Add 10 mL of Clorox and stir until the solution no longer fizzes with tiny bubbles.

4. Repeat Clorox additions with vigorous stirring after each until color of sediment changes from black to a tan/light brown/gray or completely dissolves, whichever comes first.

5. Test solution with stannous chloride for gold.

6. Do a coarse filtration on the the liquid to remove the bulk of the sediment.

7. Thoroughly rinse the sediment in the filter.

8. Perform a final fine filtration through a vacuum filter paper and a frit or with a charmin plug.

9. Heat the filtered solution on low heat to drive off any excess chlorine.

10. Add SMB to precipitate the gold.

If the material is not from a cell I may proceed differently.

Steve


Sounds like you either typed this backwards from my instructions or performed it backwards, I will assume it's a typo as you should add the HCl to the powder first, then slowly add small increments of Clorox. You may have to add more HCl if a small fresh addition of Clorox does not produce any reaction and there is still visible gold, black powder, or brown powder present. Since liquid bleach is dilute (2.5-5%) right out of the jug, not much chlorine gas (the active ingredient) is formed with each addition, that's why the fizzing stops. Stirring allows the dilute Clorox to contact the HCl in the solution to produce the chlorine gas to dissolve the gold. Stirring also brings the powder off the bottom of the beaker and allows it to contact the chlorine. This is why stirring is so important. Not just a simple stir like you stir your coffee, but repeated vigorous stirring.
 
Barren Realms 007 said:
Sounds like you either typed this backwards from my instructions or performed it backwards, I will assume it's a typo as you should add the HCl to the powder first, then slowly add small increments of Clorox. You may have to add more HCl if a small fresh addition of Clorox does not produce any reaction and there is still visible gold, black powder, or brown powder present. Since liquid bleach is dilute (2.5-5%) right out of the jug, not much chlorine gas (the active ingredient) is formed with each addition, that's why the fizzing stops. Stirring allows the dilute Clorox to contact the HCl in the solution to produce the chlorine gas to dissolve the gold. Stirring also brings the powder off the bottom of the beaker and allows it to contact the chlorine. This is why stirring is so important. Not just a simple stir like you stir your coffee, but repeated vigorous stirring.
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yea i mixed the hcl & clorox first then added the powder, then added more clorox, heated, added more clorox, more acid. Nothing. so i let it cool down & filtered the black powder, tested the liquid with stannous, which was negative. so i tossed the acid clorox & kept the powder. again i only used a small amount of powder (from the first sulfur cell run) as a test.

now i have 2.52g of black powder from the sulfur cell (not including first run) + ~1g in foils. Plus the gold still inside of the parts, which is about the same amount as the outside.

i am willing to have another go at hcl+clorox or hcl+pool shock (calcium hypochlorite). if all else fails i have the nitric for AR.

i am still wondering how to digest the rest of the parts to get to the inner gold? hot nitric has no effect, or anything else for that matter, except for AR. i would hate to throw away 2g of gold just because.

Thanks for all the help.
 
Try the HCL/clorox as Steve suggests, you will be suprised how well following his guidence works.

Your remaining items I think I would boil them in water to remove any traces of acid and then roast them to remove any traces of acid or water and then try the cell again. What were you using for your power source for your cell?
 
Barren Realms 007 said:
Try the HCL/clorox as Steve suggests, you will be suprised how well following his guidence works.

Your remaining items I think I would boil them in water to remove any traces of acid and then roast them to remove any traces of acid or water and then try the cell again. What were you using for your power source for your cell?
Click to expand...

i got a 10 amp battery charger set on manual. it never used more than 6 amps tho.

the parts are clean, externally. nice and shiny. except for a few specks here & there, nothing id put in the cell again for. it is the gold inside of them im after. they are press fit together & both sides of the press fit parts are plated, plus there is a plastic piece inside each one that is covering some gold plating too. the parts are clean and appear void of gold, but i have one that digested partially that you can see the inner gold ( http://www.mediafire.com/i/?nleaqiqzzjm ) plus the parts from the AR that didnt digest ( http://www.mediafire.com/i/?wozwgjmgni2 ) that show more foil that was missed. i did the math based on what i got from a test run of 20 parts and can estimate the internal gold content of being around 2.5g for the entire 500g.


New Photos After Hot Nitric wash:

nice and shiny:
http://www.mediafire.com/i/?4nedngom2ze

new / post sulfur cell / post hot nitric wash:
http://www.mediafire.com/i/?mzd5mw0mzzb

before & after:
http://www.mediafire.com/i/?w2znoqqo1y4

gold foil left behind after Hot Nitric wash:
http://www.mediafire.com/i/?ojnd4qmyzj5
http://www.mediafire.com/i/?wkzkr1zruqy
 
i just found out that coffee pots are not necessarily the best thing to use. turned the heat on medium & was heatin some AR up, then just as i turned the heat down the bottom of the jar cracked & started leakin hot AR into my hotplate.

luckily i had a dish nearby to pour the hot AR into so i only lost a few drops. either way i about sh*t myself.
 
Even the best lab glass can give it up with little or no warning. It pays to be ready for anything. Bring plain water to a hard boil before you trust used coffee pots. Some will last a long time but others have been subjected to too much abuse in their normal life span.
 
qst42know said:
Even the best lab glass can give it up with little or no warning. It pays to be ready for anything. Bring plain water to a hard boil before you trust used coffee pots. Some will last a long time but others have been subjected to too much abuse in their normal life span.
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yea i used it not much. i felt safer boiling with the pyrex bowl. im just glad it didnt all go at once and dump hot acid on my hotplate.

i heard it crack and thought ooh sh... then i saw it drip.... haha cat like reflexes.

these connectors are a serious pain in the ass. hell of a first time go. i shoulda tried plain pins or something simple. too bad its such an expensive hobby to learn.
 
if a glass of solution cracks it is not a good idea to lift it, the bottom can fall out, you can remove contents with suction bulb, these are also good for transferring or adding solutions as well as decanting down to the last drop. catch basin under hot plate and on workbench can aid in holding spills, cafeteria fiberglass tray's work here.

http://www.google.com/imgres?imgurl=http://images.allegrocentral.com/A9/C1/50cc-ml-Irrigation-Bulb-Syringe-560327-MEDIUM_IMAGE.jpg&imgrefurl=http://www.allegromedical.com/syringes-c570/50cc-ml-irrigation-bulb-syringe-p560327.html&usg=__DLXtYhn9j6dRLpwsr8KTEioi-M4=&h=240&w=240&sz=6&hl=en&start=13&um=1&itbs=1&tbnid=D9i9HL0O0rrccM:&tbnh=110&tbnw=110&prev=/images%3Fq%3Dsuction%2Bbulb%2Bsyringe%26um%3D1%26hl%3Den%26sa%3DN%26tbs%3Disch:1

http://www.google.com/imgres?imgurl=http://www.1-hydroponics.co.uk/images/miscellaneous/middlesize/pipettes.jpg&imgrefurl=http://www.1-hydroponics.co.uk/miscellaneous.htm&usg=__cRQnFnNa_qRrVc5yPjrtH0KmoFM=&h=248&w=357&sz=11&hl=en&start=81&um=1&itbs=1&tbnid=6b1T7q2OlBuCxM:&tbnh=84&tbnw=121&prev=/images%3Fq%3Dsuction%2Bbulb%2Bpipette%26start%3D80%26um%3D1%26hl%3Den%26sa%3DN%26ndsp%3D20%26tbs%3Disch:1
 
One thing that struck me while reading your post is that you mixed the HCl and Clorox, then added more Clorox. You tested the resulting solution for gold using stannous chloride and it showed negative. When you test the solution for gold you must ensure that all the chlorine has been gassed off by heating or by exposing to sunlight and/or open air, preferably overnight. If you hurry that step the solution will immediately redissolve your gold giving the false impression that you have a negative test. It's possible you tossed some or all of your values with the solution when it seemed to test negative.

I hope I'm wrong!
 
eveything one can possibly need to grow some good chronic .thanks for the link butcher :lol: :lol: :mrgreen:
 
gold4mike said:
One thing that struck me while reading your post is that you mixed the HCl and Clorox, then added more Clorox. You tested the resulting solution for gold using stannous chloride and it showed negative. When you test the solution for gold you must ensure that all the chlorine has been gassed off by heating or by exposing to sunlight and/or open air, preferably overnight. If you hurry that step the solution will immediately redissolve your gold giving the false impression that you have a negative test. It's possible you tossed some or all of your values with the solution when it seemed to test negative.

I hope I'm wrong!
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thats a good tip, thanks. i weighed the black powder before & after putting it into the hcl+clorox & it was the same. when i put it in nothing happened. when i heated it, nothing happened. it felt rather disappointing. i still have about 3 grams of foil/black powder (from sulfur cell) that needs taken care of.

what color is the black powder usually After running it threw hcl+clorox??

btw i tried to AR the remaining parts to get the inner gold since nothing else would digest them, this time the AR failed. it barely digested anything. the first time it completely digested the very same parts. i even heated it this time!

what a mess.
 
gold4mike said:
One thing that struck me while reading your post is that you mixed the HCl and Clorox, then added more Clorox. You tested the resulting solution for gold using stannous chloride and it showed negative. When you test the solution for gold you must ensure that all the chlorine has been gassed off by heating or by exposing to sunlight and/or open air, preferably overnight. If you hurry that step the solution will immediately redissolve your gold giving the false impression that you have a negative test. It's possible you tossed some or all of your values with the solution when it seemed to test negative.

I hope I'm wrong!
Click to expand...
I agree with this .And now you have ether sliver chlorides(if they used silverplate and i think they did) or lead sulfates as your black powder never throw away any thing untill you have what you're after.
also the term "to completion" is very important ,you may have to add more acid or oxidizer so you can go to completion
 

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