AP Waste Solution will not clear - dirty transmission oil

[Rattlerant]

Hi Forum,

Introductions first as this is my first post.

I live in Ontario Canada. I collected old servers and computers for 7 years and spent days stripping them down. I ended up with about 3 lbs of mixed low-grade pins and 3 lbs of trimmed fingers.
With the help of this forum and Streetips Videos i successfully extracted and refined a .999 3.4 gram gold button. I think this is a good yield for what i started with based on estimates throughout this forum.

Now here is the issue:

I want to clean my AP solution for next use but it's being stubborn - and i'm not a patient person.

Here are the details - hoping i don't forget anything:

(I have the spent AP solution in a separate bucket from my spent Aqua Regia - for this post, i'm only focusing on the cleanup of the spent AP solution.)

*** Edit ***
Mystery solved
after Shark and Moderator pointed out something - i messed up - i combined my AP (HCL+H2o2) solution with sufuric from my Cell
***********

• The 2 liters of Sulfuric Acid and Peroxide are in their own bucket - no other acids or chemicals were added into this waste bucket - a bit of water was added during the rinses
• 1 liter of Sulfuric acid was used to make AP to strip fingers
• 1 liter of Sulfuric acid was used as electrolyte to electro-strip the pins in a stripping cell
• All sulfuric waste went into this one bucket
• bubbler (without stone) is in the bucket
• 2 weeks ago i put 2 @ 6" copper pipes in there to cement out - it ate the copper completely so i added more copper
• 1 week ago I got impatient and added two (degreased) iron railway spikes to simply cement everything out - there is now some precipitate on them
• AP solution still looks like dirty red transmission oil
• If i dilute the AP solution with water to 50/50 mix in plastic spoon, it goes slightly green but still dirty red/brown
• adding drops of water to the bucket results in a slight white cloud
• Stannous chloride test shows no PMs in solution - strip is completely clear after 3 seconds
• if i take a drop of AP solution in a plastic spoon and drop HCL into it, after about 5 drops of HCL it still does not clear completely - only a bit - still brown dirty

Here are some things (mistakes?) that may have contributed to this:

• My Sulfuric acid drain cleaner was not clear - it was red - the MSDS for it states 60-100% concentrated sulfuric acid - and nothing else ... mystery additive to make it red?
  • Here is link to the product: https://www.homehardware.ca/en/1l-fast-acting-drain-cleaner/p/4520052
  • I tried to concentrate it more by boiling down for a day but it didn't boil down - it actually increased in volume slightly ... so i'm assuming it's close to 100%
• Also - to start the AP, I had some 30% hydrogen peroxide from a different experiment (not 3%) so i used it ... probably about 1 part peroxide to 5 parts sulfuric acid
• I have read that with a 3:1 concentrated sulfuric acid (H2SO4) to 30% hydrogen peroxide (aqueous H2O2) solution, you get 'piranha etch' - and can dissolve your gold
  • ... so this is why i want to just cement everything out an re-refine the metals to see what PMGs i may have missed - and perhaps get a bit of silver

The questions:

- How can i get my AP back to green?
- Do i just need more patience?
- Even though my yield seems good ... I most likely dissolved some gold in the 'piranha etch' - right?

Thanks to you all for the great information. And thanks in advance for any assistance.

 

[Shark]

1 liter of Sulfuric acid was used to make AP to strip fingers

The is no sulfuric in AP. It is made using Hydrochloric acid and maybe, peroxide. Better yet use HCl and an aquarium pump to supply the extra oxygen in place of the peroxide.

 

[Yggdrasil]

Hi Forum,

Introductions first as this is my first post.

I live in Ontario Canada. I collected old servers and computers for 7 years and spent days stripping them down. I ended up with about 3 lbs of mixed low-grade pins and 3 lbs of trimmed fingers.
With the help of this forum and Streetips Videos i successfully extracted and refined a .999 3.4 gram gold button. I think this is a good yield for what i started with based on estimates throughout this forum.

Now here is the issue:

I want to clean my AP solution for next use but it's being stubborn - and i'm not a patient person.

Here are the details - hoping i don't forget anything:

(I have the spent AP solution in a separate bucket from my spent Aqua Regia - for this post, i'm only focusing on the cleanup of the spent AP solution.)

• The 2 liters of Sulfuric Acid and Peroxide are in their own bucket - no other acids or chemicals were added into this waste bucket - a bit of water was added during the rinses
• 1 liter of Sulfuric acid was used to make AP to strip fingers
• 1 liter of Sulfuric acid was used as electrolyte to electro-strip the pins in a stripping cell
• All sulfuric waste went into this one bucket
• bubbler (without stone) is in the bucket
• 2 weeks ago i put 2 @ 6" copper pipes in there to cement out - it ate the copper completely so i added more copper
• 1 week ago I got impatient and added two (degreased) iron railway spikes to simply cement everything out - there is now some precipitate on them
• AP solution still looks like dirty red transmission oil
• If i dilute the AP solution with water to 50/50 mix in plastic spoon, it goes slightly green but still dirty red/brown
• adding drops of water to the bucket results in a slight white cloud
• Stannous chloride test shows no PMs in solution - strip is completely clear after 3 seconds
• if i take a drop of AP solution in a plastic spoon and drop HCL into it, after about 5 drops of HCL it still does not clear completely - only a bit - still brown dirty

Here are some things (mistakes?) that may have contributed to this:

• My Sulfuric acid drain cleaner was not clear - it was red - the MSDS for it states 60-100% concentrated sulfuric acid - and nothing else ... mystery additive to make it red?
  • Here is link to the product: https://www.homehardware.ca/en/1l-fast-acting-drain-cleaner/p/4520052
  • I tried to concentrate it more by boiling down for a day but it didn't boil down - it actually increased in volume slightly ... so i'm assuming it's close to 100%
• Also - to start the AP, I had some 30% hydrogen peroxide from a different experiment (not 3%) so i used it ... probably about 1 part peroxide to 5 parts sulfuric acid
• I have read that with a 3:1 concentrated sulfuric acid (H2SO4) to 30% hydrogen peroxide (aqueous H2O2) solution, you get 'piranha etch' - and can dissolve your gold
  • ... so this is why i want to just cement everything out an re-refine the metals to see what PMGs i may have missed - and perhaps get a bit of silver

The questions:

- How can i get my AP back to green?
- Do i just need more patience?
- Even though my yield seems good ... I most likely dissolved some gold in the 'piranha etch' - right?

Thanks to you all for the great information. And thanks in advance for any assistance.

Welcome.
You need to study more since you have your information mixed up.
As Shark said the AP is actually a Cupric Chloride leach where the Copper is dissolved from under the foils.
And AP is really never spent, it lives "forever" as long as it is not contaminated.

 

[Yggdrasil]

Hi Forum,

Introductions first as this is my first post.

I live in Ontario Canada. I collected old servers and computers for 7 years and spent days stripping them down. I ended up with about 3 lbs of mixed low-grade pins and 3 lbs of trimmed fingers.
With the help of this forum and Streetips Videos i successfully extracted and refined a .999 3.4 gram gold button. I think this is a good yield for what i started with based on estimates throughout this forum.

Now here is the issue:

I want to clean my AP solution for next use but it's being stubborn - and i'm not a patient person.

Here are the details - hoping i don't forget anything:

(I have the spent AP solution in a separate bucket from my spent Aqua Regia - for this post, i'm only focusing on the cleanup of the spent AP solution.)

• The 2 liters of Sulfuric Acid and Peroxide are in their own bucket - no other acids or chemicals were added into this waste bucket - a bit of water was added during the rinses
• 1 liter of Sulfuric acid was used to make AP to strip fingers
• 1 liter of Sulfuric acid was used as electrolyte to electro-strip the pins in a stripping cell
• All sulfuric waste went into this one bucket
• bubbler (without stone) is in the bucket
• 2 weeks ago i put 2 @ 6" copper pipes in there to cement out - it ate the copper completely so i added more copper
• 1 week ago I got impatient and added two (degreased) iron railway spikes to simply cement everything out - there is now some precipitate on them
• AP solution still looks like dirty red transmission oil
• If i dilute the AP solution with water to 50/50 mix in plastic spoon, it goes slightly green but still dirty red/brown
• adding drops of water to the bucket results in a slight white cloud
• Stannous chloride test shows no PMs in solution - strip is completely clear after 3 seconds
• if i take a drop of AP solution in a plastic spoon and drop HCL into it, after about 5 drops of HCL it still does not clear completely - only a bit - still brown dirty

Here are some things (mistakes?) that may have contributed to this:

• My Sulfuric acid drain cleaner was not clear - it was red - the MSDS for it states 60-100% concentrated sulfuric acid - and nothing else ... mystery additive to make it red?
  • Here is link to the product: https://www.homehardware.ca/en/1l-fast-acting-drain-cleaner/p/4520052
  • I tried to concentrate it more by boiling down for a day but it didn't boil down - it actually increased in volume slightly ... so i'm assuming it's close to 100%
• Also - to start the AP, I had some 30% hydrogen peroxide from a different experiment (not 3%) so i used it ... probably about 1 part peroxide to 5 parts sulfuric acid
• I have read that with a 3:1 concentrated sulfuric acid (H2SO4) to 30% hydrogen peroxide (aqueous H2O2) solution, you get 'piranha etch' - and can dissolve your gold
  • ... so this is why i want to just cement everything out an re-refine the metals to see what PMGs i may have missed - and perhaps get a bit of silver

The questions:

- How can i get my AP back to green?
- Do i just need more patience?
- Even though my yield seems good ... I most likely dissolved some gold in the 'piranha etch' - right?

Thanks to you all for the great information. And thanks in advance for any assistance.

Where did you find the information on using Sulfuric for AP?
This is a puzzle and I'm confident it was not with SreeTips.

Here is something to study:
We ask our new members to do 3 things.
1. Read C.M. Hokes book on refining jewelers scrap, it gives an easy introduction to the most important chemistry regarding refining.
It is free here on the forum: https://goldrefiningforum.com/phpBB3/viewtopic.php?f=54&t=19798
2. Then read the safety section of the forum: https://goldrefiningforum.com/forums/safety.47/
3. And then read about "Dealing with waste" in the forum: https://goldrefiningforum.com/threads/dealing-with-waste.10539/

Suggested reading:
https://goldrefiningforum.com/forums/the-library.101/
https://goldrefiningforum.com/threads/when-in-doubt-cement-it-out.30236/
https://goldrefiningforum.com/threa...le-read-this-before-you-post-about-ore.33333/


Forum rules is here.
https://goldrefiningforum.com/threads/gold-refining-forum-rules.31182/

 

[Rattlerant]

Welcome.
You need to study more since you have your information mixed up.
As Shark said the AP is actually a Cupric Chloride leach where the Copper is dissolved from under the foils.
And AP is really never spent, it lives "forever" as long as it is not contaminated.

Yggdrasil,

Thank-you for jogging my memory. I realized what i did now. (old man memory).

I had 1 litre of AP (HCL+H2o2) and i added the 2 liters of sulfuric acid from my electro-stripping cell to the same bucket! DUGH!
I see now that the volume in the bucket is about 3 liters. Wow - i need a nap.

No wonder it's not coming clean!

So, i'm assuming this has to be treated and discarded now - right?
Will the steel spikes still precipitate the metals?

 

[Rattlerant]

The is no sulfuric in AP. It is made using Hydrochloric acid and maybe, peroxide. Better yet use HCl and an aquarium pump to supply the extra oxygen in place of the peroxide.

Thanks - i realize what i did now and added a *** edit *** to the post.

 

[Rattlerant]

Where did you find the information on using Sulfuric for AP?
This is a puzzle and I'm confident it was not with SreeTips.

Here is something to study:
We ask our new members to do 3 things.
1. Read C.M. Hokes book on refining jewelers scrap, it gives an easy introduction to the most important chemistry regarding refining.
It is free here on the forum: https://goldrefiningforum.com/phpBB3/viewtopic.php?f=54&t=19798
2. Then read the safety section of the forum: https://goldrefiningforum.com/forums/safety.47/
3. And then read about "Dealing with waste" in the forum: https://goldrefiningforum.com/threads/dealing-with-waste.10539/

Suggested reading:
https://goldrefiningforum.com/forums/the-library.101/
https://goldrefiningforum.com/threads/when-in-doubt-cement-it-out.30236/
https://goldrefiningforum.com/threa...le-read-this-before-you-post-about-ore.33333/


Forum rules is here.
https://goldrefiningforum.com/threads/gold-refining-forum-rules.31182/

I did 1 2 3 ... have been researching this for 7 years - read almost everything on this forum dealing with gold refining. I'm jut forgetful i guess Thanks for the assistance.

 

[Yggdrasil]

I did 1 2 3 ... have been researching this for 7 years - read almost everything on this forum dealing with gold refining. I'm jut forgetful i guess Thanks for the assistance.

Then you will need to concentrate.
These kind of mistakes can kill you if it is other substances or you are unlucky.
In a chemical lab we simply can not afford too much slip of mind.

 

[galenrog]

The best way to avoid this in the future is to do tho things. 1: Label all items, regardless of how inconsequential they may seem. 2: Prior to any procedure, work up a flow chart or similar set of instructions before you start, and follow those instructions.

Doing these two things help me immensely regardless of the task, and save an immense amount of time should something unusual be encountered.

Time for more coffee.

 

[Rattlerant]

The best way to avoid this in the future is to do tho things. 1: Label all items, regardless of how inconsequential they may seem. 2: Prior to any procedure, work up a flow chart or similar set of instructions before you start, and follow those instructions.

Doing these two things help me immensely regardless of the task, and save an immense amount of time should something unusual be encountered.

Time for more coffee.

This is good advice. Thanks.

I did label everything except the sulfuric acid and at 2am I made the mistake of pouring it into my AP waste and went to bed. No more late night chemistry for me

I'm going to neutralize, use iron to drop metals, filter and dispose of solutions. Re-refine the filtered particulates at a later date. Does this sound like the correct approach?

 

[Yggdrasil]

This is good advice. Thanks.

I did label everything except the sulfuric acid and at 2am I made the mistake of pouring it into my AP waste and went to bed. No more late night chemistry for me

I'm going to neutralize, use iron to drop metals, filter and dispose of solutions. Re-refine the filtered particulates at a later date. Does this sound like the correct approach?

Not too bad, but try to follow the waste protocol.
You need to push the pH up to around 10/11 ish if I remember correct, then filter and lower the pH more and filter again.
It is all in the waste thread.
It has to do with the solubility of the different Hydroxides.

 

[anachronism]

This is good advice. Thanks.

I did label everything except the sulfuric acid and at 2am I made the mistake of pouring it into my AP waste and went to bed. No more late night chemistry for me

I'm going to neutralize, use iron to drop metals, filter and dispose of solutions. Re-refine the filtered particulates at a later date. Does this sound like the correct approach?

You hit the nail firmly on the head here Rattle. As sure as eggs are eggs the ONE thing you don't label is the one thing that causes you issues. I feel your pain. Deeply.

 

[4metals]

And, avoid abbreviations on your labels. And read the entire label! I had a worker once who mixed bone ash and borax for a flux blend. what a mess. He said he read the ash part right, but it should have been soda ash.

 

[Rattlerant]

Thank

Not too bad, but try to follow the waste protocol.
You need to push the pH up to around 10/11 ish if I remember correct, then filter and lower the pH more and filter again.
It is all in the waste thread.
It has to do with the solubility of the different Hydr

Not too bad, but try to follow the waste protocol.
You need to push the pH up to around 10/11 ish if I remember correct, then filter and lower the pH more and filter again.
It is all in the waste thread.
It has to do with the solubility of the different Hydroxides.

Thanks again. I think I found the correct post. https://goldrefiningforum.com/threads/dealing-with-waste.10539/

I resign to be a more patient person. Lol. I will find the correct process.

 

[Martijn]

Thank



Thanks again. I think I found the correct post. https://goldrefiningforum.com/threads/dealing-with-waste.10539/

I resign to be a more patient person. Lol. I will find the correct process.

I understand you have AP with sulfuric.
I don't think it will harm the process much. The dark color will likely be cuprous chloride.
The sulfuric will convert some chloride salts in sulfate salts, freeing up more chloride to return to the AP cycle.
As long as no insoluble sulfates form, you should be ok. Imo.

 

[Rattlerant]

I understand you have AP with sulfuric.
I don't think it will harm the process much. The dark color will likely be cuprous chloride.
The sulfuric will convert some chloride salts in sulfate salts, freeing up more chloride to return to the AP cycle.
As long as no insoluble sulfates form, you should be ok. Imo.

Thanks for the words of wisdom and the boost in confidence. I feel pretty dumb right now. But it's all a part of learning i guess.

 

[Shark]

It would be nice if we could start at the top, but it never works that way for me.

 

[galenrog]

Thanks for the words of wisdom and the boost in confidence. I feel pretty dumb right now. But it's all a part of learning i guess.

Nearly everyone on this Forum has at least one PhD in DUMB. I have several.

Time for more coffee.

 

[Yggdrasil]

Nearly everyone on this Forum has at least one PhD in DUMB. I have several.

Time for more coffee.

True, but we still hope the new ones learn the important stuff without injuries or damage.
I have had luck more than one time