Accomplished nothing so far

[Yggdrasil]

I have a lot of questions right now. I appreciate any advice, instructions or confirmation of my plans. I’m at the point on a 300 ml test batch that’s positive for gold that I need to de-nox with sulphamic acid. Approximately how much should I use? How much water should I add to the solution? And, should I shoot for ph of 2-4? IF successful, I’ve got Ferrous Sulphate to drop gold. How long should I wait before adding the FeSO4? I’m anticipating < 0.5g gold. How much Ferrous should I add to drop that small amount? IF I get a successful gold drop should I decant or siphon before washing? Thanks very much for any help.

We need a bit more details.
How much Nitric did you use for dissolving the Gold?
The amount of free Nitric is what dictates how much if any is needed.
If you have to use Sulfamic most add it as crystals, no need to dissolve it.
No need to adjust acidity.
I assume you already have cooled and filtered before contemplating the use of Sulfamic.
If you determine to use Sulfamic just to be on the safe side,
heat the solution to almost boiling and add crystals,
make sure the container is not more than 1/3 full.
When there is no more fizzing it is done.
Filter to crystal clear and drop the Gold.

One need to use about 4 to 1 with Ferrous sulfate to Gold.
Then settle and decant/siphon well and start washing.

 

[anachronism]

To add to Yggs post whatever you do add a tiny pinch of Sulphamic to judge the reaction. No more, otherwise you're boiling the solution over.

 

[Dreamer]

No need to dilute it unless it's viscous and do so, if needed with HCl. Heat your liqour to at least 90c in a beaker no more than 1/3 full. Add the sulfamic grain wise and wait for it to calm down before adding more. The top foam sequesters the liberated Nox and drives it back into solution so try to avoid forming a head to minimize the need for excessive sulfamic. This takes a while so be patient. When you get to the point that there is minimum reaction, let it heat for another hour covered and watch for any brown gas that may form. If you're still getting the gas, continue adding sulfamic.

You want to avoid using too much because an excess clogs the filter in your next step. Once there is no more gas accumulating, filter. Filter it cold.

Reducing the acidity before precipitating is controversal here but I've had better results by doing so. Just get it off 1- thats all I do. Pushing it further risks contaminating your gold and I've found it to be no less effective than 2 or 3.

To decant or siphon is a matter of preference. I alway pour off through a filter into a jar with a copper pipe in it. Any particles will get trapped in the filter and easily rinsed back into the beaker. Any PM's in solution will cement out on the copper and you can recover those later.

I always do a cold water rinse before I do the HCl boil. After the HCl boil, do a stannous test before you pour it off! Residual nitric will dissolve (some, if not all of) your gold back into solution. If it's positive AND you have precipitant left in the beaker, than cool it off and add more precipitant then repeat the clean up steps.

Dry it up on low heat and you should be Golden.

 

[Edwin Price]

We need a bit more details.
How much Nitric did you use for dissolving the Gold?
The amount of free Nitric is what dictates how much if any is needed.
If you have to use Sulfamic most add it as crystals, no need to dissolve it.
No need to adjust acidity.
I assume you already have cooled and filtered before contemplating the use of Sulfamic.
If you determine to use Sulfamic just to be on the safe side,
heat the solution to almost boiling and add crystals,
make sure the container is not more than 1/3 full.
When there is no more fizzing it is done.
Filter to crystal clear and drop the Gold.

One need to use about 4 to 1 with Ferrous sulfate to Gold.
Then settle and decant/siphon well and start washing.

Much less nitric than before. Instead of 3:1, more like 8:1 ratio. ty

 

[Yggdrasil]

Much less nitric than before. Instead of 3:1, more like 8:1 ratio. ty

Not much detail here Edwin.
What was the material?
How did you dissolve the material?
8:1 will mean 40 ish ml Nitric?
That is enough to dissolve 40 to 60 g of Gold if it was used as AR.

 

[galenrog]

Much less nitric than before. Instead of 3:1, more like 8:1 ratio. ty

We avoid ratios of nitric to HCl. Use enough HCl to cover your material. Add nitric one or two ml at a time until material dissolved. Easy. Leads to less waste.

Time for more coffee.

 

[Edwin Price]

Not much detail here Edwin.
What was the material?
How did you dissolve the material?
8:1 will mean 40 ish ml Nitric?
That is enough to dissolve 40 to 60 g of Gold if it was used as AR.

Yes indeed. Still way too much nitric even though it was probably closer to 10:1 ratio. Every positive solution I have for gold tests crimson red with litmus paper. I tried diluting with water and adding more sulphamic acid with no change. Still tests blood red. There is no fizzing and it’s hard to dissolve the sulphamic crystals too. Should I continue to add sulphamic acid and dilute further. Should I boil off some of the acid? I know sodium bicarbonate and hydroxide are alkaline. Might it help to add any of either? I’m including pics of the ph paper scale and my actual results. I’m going about this issue slow and methodically. I don’t want to ruin my first four gold positive test solutions at this point. Thank you all for continuing to advise.

 

[Edwin Price]

Yes indeed. Still way too much nitric even though it was probably closer to 10:1 ratio. Every positive solution I have for gold tests crimson red with litmus paper. I tried diluting with water and adding more sulphamic acid with no change. Still tests blood red. There is no fizzing and it’s hard to dissolve the sulphamic crystals too. Should I continue to add sulphamic acid and dilute further. Should I boil off some of the acid? I know sodium bicarbonate and hydroxide are alkaline. Might it help to add any of either? I’m including pics of the ph paper scale and my actual results. I’m going about this issue slow and methodically. I don’t want to ruin my first four gold positive test solutions at this point. Thank you all for continuing to advise.

My solution also contains about 100 ml of water.

 

[Edwin Price]

We avoid ratios of nitric to HCl. Use enough HCl to cover your material. Add nitric one or two ml at a time until material dissolved. Easy. Leads to less waste.

Time for more coffee.

Coffee is good. Time for more Jack Daniel’s for me.

 

[Proffshuggarn]

Yes indeed. Still way too much nitric even though it was probably closer to 10:1 ratio. Every positive solution I have for gold tests crimson red with litmus paper. I tried diluting with water and adding more sulphamic acid with no change. Still tests blood red. There is no fizzing and it’s hard to dissolve the sulphamic crystals too. Should I continue to add sulphamic acid and dilute further. Should I boil off some of the acid? I know sodium bicarbonate and hydroxide are alkaline. Might it help to add any of either? I’m including pics of the ph paper scale and my actual results. I’m going about this issue slow and methodically. I don’t want to ruin my first four gold positive test solutions at this point. Thank you all for continuing to advise.

Hi Edwin
I recognize myself in the situation you are in now. It is very easy to get into a rut here and only make the situation worse, with value "locked up" in the liquid.
My advice to you now is:
-Stop, turn off the heat, cover the beaker with a loose lid and put the stuff away in safe places, until you can figure it out theoretically and practically and hopefully with a lot of guidance from the more experienced here in which part of the process it went "wrong". It's not sugar cake you bake right away.

-If you want professional help out of the situation (which can be solved), then answer the professional's questions (eg Yggdrasil at the latest).

- Details! How many ml of this and that, what exactly are you processing and so on. Without these facts it is impossible/very difficult to help you.

This is a "big" pinch of Sulfamic acid at the end of an ice cream stick, maybe 0.2g... I usually start the "degassing" with half that amount.
Like half the little finger nail. Often enough

/Dennis

 

[Edwin Price]

Yes indeed. Still way too much nitric even though it was probably closer to 10:1 ratio. Every positive solution I have for gold tests crimson red with litmus paper. I tried diluting with water and adding more sulphamic acid with no change. Still tests blood red. There is no fizzing and it’s hard to dissolve the sulphamic crystals too. Should I continue to add sulphamic acid and dilute further. Should I boil off some of the acid? I know sodium bicarbonate and hydroxide are alkaline. Might it help to add any of either? I’m including pics of the ph paper scale and my actual results. I’m going about this issue slow and methodically. I don’t want to ruin my first four gold positive test solutions at this point. Thank you all for continuing to advise.

Not much detail here Edwin.
What was the material?
How did you dissolve the material?
The source material was gold plated computer parts and some actual gold ore crushed to a powder. It was placed in a 1000 ml beaker. The material was cover in HCL. Then an equivalent amount of water was added. It was heated, with a strong reaction for 30 minutes and filtered. Remnants of any plastic, fiberboard, waste, etc. were removed. The solute was washed multiple times. Then the solution and solute were recombined. More HCL was added along with about 3 pippetes of Nitric - maybe 20ml. The mixture was again heated till a vigorous action occurred - total about 30 minutes. Afterwards, the solution was filtered and cooled. It tested positive (black) for gold.

 

[Proffshuggarn]

The source material was gold plated computer parts and some actual gold ore crushed to a powder.

And that is a perfect example..
What kind of “gold plated computer parts?!
-Details!
I’m not laughing at you, I’m suffering with you because I know how it feels in this situation.

Just trying to help you
/Dennis

 

[Edwin Price]

Hi Edwin
I recognize myself in the situation you are in now. It is very easy to get into a rut here and only make the situation worse, with value "locked up" in the liquid.
My advice to you now is:
-Stop, turn off the heat, cover the beaker with a loose lid and put the stuff away in safe places, until you can figure it out theoretically and practically and hopefully with a lot of guidance from the more experienced here in which part of the process it went "wrong". It's not sugar cake you bake right away.

-If you want professional help out of the situation (which can be solved), then answer the professional's questions (eg Yggdrasil at the latest).

- Details! How many ml of this and that, what exactly are you processing and so on. Without these facts it is impossible/very difficult to help you.

This is a "big" pinch of Sulfamic acid at the end of an ice cream stick, maybe 0.2g... I usually start the "degassing" with half that amount.
Like half the little finger nail. Often enough
View attachment 62183
/Dennis

Understand. But I’d like to correct the problem with this batch now. I know there’s gold present, I used far less nitric, I’m using sulphamic acid as advised. But the solution appears way too acidic to try add ferrous sulfate and drop the gold at this point. I’ve read the ph between 2-4 is the desirable range that I need to achieve. ty

 

[Edwin Price]

Not much detail here Edwin.
What was the material?
How did you dissolve the material?

Answer: Gold fingers, pins and wire.

 

[Proffshuggarn]

Answer: Gold fingers, pins and wire.

What kind of pins (magnetic?) and wire?
Ok, I'll give it a try..
-You poured an unknown amount of Hcl and an equal amount of water over the mixed material.
(You then dissolved some junk and base metals)

-You filtered the contaminated Hcl/H2O solution and separated the residual material from the liquid, and washed the material.
(And here after I think the problem arose)

-You put the washed material back into the contaminated Hcl/H2O solution.

-You topped up the contaminated liquid with an unknown amount of new Hcl and then started adding nitric acid.

Have I understood you correctly?

-My understanding is that your solution was already saturated with base metals and unknown other substances from your first Hcl/H2O solution and also too dilute to be suitable for AR.

We usually do AR with concentrated Hcl (do not add water) and drip in ml by ml of concentrated nitric until no more reaction occurs, then check if there is excess nitric acid left.
And this is where my knowledge ends..

I know there are ways to save your values, evaporation and more.. However, I don't know this well enough to guide you through it.
/Dennis

 

[Edwin Price]

What kind of pins (magnetic?) and wire?
Ok, I'll give it a try..
-You poured an unknown amount of Hcl and an equal amount of water over the mixed material.
(You then dissolved some junk and base metals)

-You filtered the contaminated Hcl/H2O solution and separated the residual material from the liquid, and washed the material.
(And here after I think the problem arose)

-You put the washed material back into the contaminated Hcl/H2O solution.

-You topped up the contaminated liquid with an unknown amount of new Hcl and then started adding nitric acid.

Have I understood you correctly?

-My understanding is that your solution was already saturated with base metals and unknown other substances from your first Hcl/H2O solution and also too dilute to be suitable for AR.

We usually do AR with concentrated Hcl (do not add water) and drip in ml by ml of concentrated nitric until no more reaction occurs, then check if there is excess nitric acid left.
And this is where my knowledge ends..

I know there are ways to save your values, evaporation and more.. However, I don't know this well enough to guide you through it.
/Dennis

Pretty much correct. I used nothing magnetic. It took about 150-200 ml of HCL to cover everything. I added the equivalent amount of water. I heated for 30 mins while vigorous reaction took place. Then I filtered the solution and washed the solute. Afterwards I reused the clear green/yellow solution and added about 100 mil of HCL plus about 20 ml of Nitric during reheat till about 300 ml total solution remained. After filtering the solute, the liquid tested dark black for gold with stannous chloride. ty

 

[Edwin Price]

What kind of pins (magnetic?) and wire?
Ok, I'll give it a try..
-You poured an unknown amount of Hcl and an equal amount of water over the mixed material.
(You then dissolved some junk and base metals)

-You filtered the contaminated Hcl/H2O solution and separated the residual material from the liquid, and washed the material.
(And here after I think the problem arose)

-You put the washed material back into the contaminated Hcl/H2O solution.

-You topped up the contaminated liquid with an unknown amount of new Hcl and then started adding nitric acid.

Have I understood you correctly?

-My understanding is that your solution was already saturated with base metals and unknown other substances from your first Hcl/H2O solution and also too dilute to be suitable for AR.

We usually do AR with concentrated Hcl (do not add water) and drip in ml by ml of concentrated nitric until no more reaction occurs, then check if there is excess nitric acid left.
And this is where my knowledge ends..

I know there are ways to save your values, evaporation and more.. However, I don't know this well enough to guide you through it.
/Dennis

Got it. I should not have re-used the contaminated HCL and water solution.

 

[Shark]

Got it. I should not have re-used the contaminated HCL and water solution

When removing base metals with acids you don’t want to add the dissolved base metals back into your gold. When dropping from a dirty solution often some of the base metals will come down with the gold when doing the precipitating process. This means possibly more work in the washing processes and maybe a lower percentage of purity in the resulting button or bar. Since the recovered gold foils or powders are well reduced in size and volume, fresh acids for the refining step will be much less as well. When I first started and was experimenting I often did refines in double shot glasses. There wasn’t much gold, but there wasn’t much to lose either. And much of what I learned really aided me later.

 

[goldshark]

Not much detail here Edwin.
What was the material?
How did you dissolve the material?
The source material was gold plated computer parts and some actual gold ore crushed to a powder. It was placed in a 1000 ml beaker. The material was cover in HCL. Then an equivalent amount of water was added. It was heated, with a strong reaction for 30 minutes and filtered. Remnants of any plastic, fiberboard, waste, etc. were removed. The solute was washed multiple times. Then the solution and solute were recombined. More HCL was added along with about 3 pippetes of Nitric - maybe 20ml. The mixture was again heated till a vigorous action occurred - total about 30 minutes. Afterwards, the solution was filtered and cooled. It tested positive (black) for gold.

Was the crushed ore panned to a concentrate? Were there other components to the ore such as sulphides, and/or Manganese, and possibly some other metals? How much do you know about mineralogy?

 

[anarxi]

damn it,
why make a vinaigrette out of different golds?
Is there any gold in your ore at all?

PS
here on the forum there is a story about how people were poisoned by arsenic contained in ore during chemical processes

You were advised to buy a scrap of real gold, go through all the processes on it, and then start working on complex objects.