Uh oh... Another wierd gold drop..

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Xydoman

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Joined
May 10, 2021
Messages
33
So you guys have been absolutely essential for me drop after drop, as there seem to be anomalies with all of them lol. I want yall to know how I consider the knowledge possessed by the members of this forum to be invaluable and I'm extremely grateful to have yall to turn to.. So, now that all the mushy stuff is out of the way... here's another one :

Had a successful, yet small drop, with the powder still in the beaker that I used hcl and bleach to dissolve the gold, and smb to precipitate it after filtering.. This beaker was set aside as I worked on the next batch. Remember this beaker..

So the next batch was my first batch ever using bone fide 70% nitric acid from ebay. Here are the steps I took.. I know there is a misstep in here and you'll surely see it as well. I would like to know how to handle the results of the misstep. Yall haven't steered me wrong yet lol.

1)scrap consisted of trim ram fingers, about 150 grams, and several fully plated boards from 2 satellite dishes and 4 sound cards. The boards were completely depopulated, to where you could run your fingers over them and not catch anything with your skin. The sound cards were treated with lye to remove the solder mask. Oh, and 2 boards from hospital bed controllers that had alot of plating, and were also completely depopulated.

This was treated for 2 days in hcl and peroxide with a bubbler, changing out the dirty solution for fresh AP after day 1. The foils loose at this time were left in the bucket that I rinced them into, containing the used solution that had freed them from the scrap.

2) day 2, removed the rest of the foils and combined them with the others in the bucket with the used solution. I used distilled water to spray the foils off of the scrap and the beaker they were treated in. I now had a TON of foils, in used AP solution, a bit of distilled water, all sitting in a single bucket. I filtered them from the used ap solution and, if I had to guess, I'd say I had 7 or 8 really healthy teaspoons full of foils. Possibly more. It was gorgeous.

3) I added about 300ml of fresh hcl..( Although, noteworthy is the fact that I ran out of the Klean Strip muriatic acid that I usually use, and only had HDX that I had bought a month or so ago, that comes in a "balancing kit for swimming pools".. I assumed it was the same stuff, but a bit weaker. 20% I think, compared to the 32% of Klean strip.) I carefully and quite timidly removed a liter of 70% nitric from its shipping vessel, and quietly hoped I would soon graduate to the next level on my gold recovery skill set lol... As if.. Over the course of the next 2 hours I added 30 ml of nitric acid, 10 ml at a time.. I stopped after the 3rd dose. I still saw a few foils bouncing up and down, but not many, so I assumed this was enough. The solution was a deep orange yellow color. With bleach, the solution is usually a bright yellow, this was much darker.

3) I allowed it to do its thing for about 24 hrs, then confronted the solution. A ph test showed a solid 1, so I knew I couldn't drop it with smb yet. I guessed I used too much nitric. So I grabbed the aforementioned beaker that was set aside from the previous batch, and added it, hoping to use the remaining nitric. An odd note here, is that about half of my gold from this batch,)(which I had on a warmer for a couple of days) was stuck to the side of the glass. My spray bottle was powerless to free it, so I ended up literally scrubbing it off with about 10 qtips, and really only freeing about 80 percent of what was stuck, and I added the qtips to the AR.

4) to deal with the remaining stuck gold powder, I poured the new AR with the contents of the qtips and both batches, into the Glass with the stuck powder, in an effort to dissolve it off of the sides.. That worked. A stannous test gave an immediate indication of a heavily pregnant solution. I watched as it snapped to purple, then dark purple, then darker till it was nearly black. I now had a pregnant solution with a deep orange color and nothing stuck to the side of the glass. The qtips were reduced to sticks.

5) I filtered the gold impregnated solution into a fresh beaker. I didn't have a way to check ph at this time, so I rolled the dice. I added a couple of teaspoons of smb to about 30 or 40 ml of distilled water and disdolved it. I then stirred this into the AR solution. I watched as the solution turned from deep orange, to a muddy brown.. Then my excitement was dashed as it turned back into deep orange moments later.. I stirred up the same quantity of smb and repeated the step. And again, it changed to muddy brown for a moment, then right back to the orange. I had to leave for work.

6) at work I was researching how to correct this, and stumbled on a post about urea.. I actually have some I boutght previously. So I got home, and added what seemed like quite a bit. The last spoonful produced no reaction. Not only that, but many of the crystals settled to the bottom. The solution was now a lemon orange color. I had to wind down for bed soon, so I went ahead and added a small snout of smb without dissolving it first. Maybe a teaspoon? I went to bed and woke up today. The result here, Is a bottom layer of white stuff.. Urea? Smb? Some other precipitate? Probably about 2 mm thick? On top of that is my gold. A pretty thin layer of what looks like dirt or cinniman... And then the solution of course filling the rest of the container.

So I basically need to know how to seperate the layers, and how to correct anything in the process that I did incorrectly so that I dont repeat the same mistakes moving forward. I feel like I have described the entire chain of events pretty accurately so hopefully you can look through my eyes as I'm doing this, and just let me know what you're shaking your head and face-palming about as I'm doing it. Thanks everyone. I sure can't do this without yall.
 

Palladium

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Joined
Jan 17, 2008
Messages
5,582
Location
USA
Your going to have to do a 2nd drop anyways. Test with Stannous to make sure it is negative, then decant and redissolve. If this would have been your 2nd drop then the excess salt formed from to much over saturation would be washed away by the water washes and hcl washes. Some of what you may be seeing is more than likely silver chlorides that carried over also, but you can't tell it from all the other salts.

On to the 2nd refine!
 

Xydoman

Active member
Joined
May 10, 2021
Messages
33
Oooh I see!! Say.. If it were silver chloride, how might I recover the silver? I'll bet there's probably something on it in the forum. Thanks! I hope it is. I've been wanting to run into some ever since I took a 2 liter bottle of a milky solution to thr disposal facility. I had no idea at that time what was in it. It wasn't till much later where I watched a video explaining the milky appearance of silver chloride.. I was like... DOH!!
 

1mysurveymail

Well-known member
Joined
Sep 11, 2013
Messages
48
QUICK TIP.

Sounds like Silver Chloride. Just shooting from the hip, unless some braying thing needs a scope's reticle.

You said "urea." Sounds expensive, why not use grout cleaner = sulfamic acid from the hardware store to "DENOX" your AR? As someone encouraging you would say, "don't worry, the gold is still in there." I might take something beyond my ken, but it is still in there.

NEVER allow or ADD any extra water (not already in your 20-36% HCl) into your AP. It causes TIN/Sn to come out of solution (grey mud). Figure out a filtering and rinsing process for your gold / AP that DOES NOT ADD WATER = raises the Ph of your AP. This plagued me mightily at the start of my recovery processes, and it took a generous, forthright, straight shooting, knowledgeable contributor here (Geo the Grey Wizard) to point out the flawed steps in my recovery processes.

Meanwhile Saruman in his Ivory Tower (Orthanc) was too busy staring into his Palantir, and kept invoking some ancient tome written before modern COMPUTER alloys entered the mix. LOTR reference added for extra harshness.

The long and the short of it is that E-scrap has been Lead/Pb free since the 1980's. "Solder" is comprised of tin/Sn and perhaps some silver and some other element that escapes recollection. So the SOURCE determines the pesky bits. Repeated refines, and washes will get it done.

Quick tip,
 

jadedalex

Active member
Joined
Feb 20, 2017
Messages
43
Xydoman, you wrote:
just let me know what you're shaking your head and face-palming about as I'm doing it.
I'll say this again. you are trying to "Refine". Stop adding things to your mix. you are only making your life harder. Garbage in, Garbage out. And yes, SIlver will reek havoc with your drops. Keep reading the Library, search the Archived threads for your topic of interest and keep learning...
 

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