I can't tell if I messed up or what???

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anachronism said:
You can take out the silver and the copper with hot concentrated washes of HCl. There are conflicting opinions on the forum with regards to temperature, however I've always favoured hot. Yes it opens the door to a tiny dissolution of gold however this harks back to my comments regarding the quantity of gold you are trying to refine and the economies of scale.

I have never ever put gold powder in a filter and I don't understand the logic of doing so to be honest. It seems like a pointless exercise to me.

That would definitely be the reason copper and silver were still in there. I should have used hot rinses.

My mistake, I should have instead said, that I didn't filter it the final time while the gold was still "in solution", like I normally would to catch any trash, solid pieces, or AgCl.

About the tiny bead, I meant that I wasn't going to re-refine it "by itself". I have more material that I'm processing and will be adding it to process along with the bead when it's finished.

I'll be sure to properly do the rinses/filtering next time and possibly, finally get my first 999 gold.
 
Thanks for clarifying Grelko.

What kind of filtration are you using? If you cannot read a newspaper through the solution in total clarity then there's a very good chance that you still have silver chloride particles in your AR. Good filtration is an absolute "must have" and the vast majority of AgCl can be removed this way.
 
It also pays to allow your solution to settle well before the final filtration to allow any chloride to settle on the bottom which can take time and the simple trick of putting your solution through the same filter twice works well with catching small particles.
 
anachronism said:
Thanks for clarifying Grelko.

What kind of filtration are you using? If you cannot read a newspaper through the solution in total clarity then there's a very good chance that you still have silver chloride particles in your AR. Good filtration is an absolute "must have" and the vast majority of AgCl can be removed this way.


Edit - After I filter my solutions, I have a problem with squeezing the last drop or 2 out of the filter. This would force material through the coffee filters and dirty up the solution again. I need to stop doing that.

I'm using coffee filters for now. Depending where I am in the process, I might use 3 or 4.

Since I didn't filter it that final time, once I dropped the gold out, I made sure and decanted it until it was completely clear, no haze at all. (I normally rinse it until it's completely clear)

Just to make sure that everyone knows, I'm not using AR to dissolve, just HCl/Cl. I still haven't tried using nitric yet. I probably won't until I have a proper lab set up and I have no idea when that'll be.

nickvc said:
It also pays to allow your solution to settle well before the final filtration to allow any chloride to settle on the bottom which can take time and the simple trick of putting your solution through the same filter twice works well with catching small particles.

When I put gold into solution with HCl/Cl, I'd give it half a day or more (sometimes a few days if I'm busy), filter, then evaporate about 50% to make sure the CL is out before adding SMB.

I'm thinking that when I accidently evaporated the solution dry, whatever was still in it dropped out when I added Dwater to it, since it would be close to neutral. I should have added HCl instead.

I'll remember to run the solution through the same filter twice for certain parts, especially at the end, or if it was very dirty to start with, thanks for the idea.
 
I'm wondering if anyone could shed some light on this for me? I've been trying to find an answer on here for the last few days.


In the first jar was, the dirty gold powder from the original button that I dissolved in this thread. I had kept it in a mason jar for a while, still in the solution it was precipitated in. The lid rusted and iron possibly got into it. (approx 0.7g dirty powder, that came from IC chips)

I had a second jar with AP in it (lid rusted also, possible iron), that had approx 31g of mixed material.

The material/powder in the second jar, started out as a mix of...

9g of dirty powder left over from ~4lbs plated pins
~1g from ~3/4 pound gold fingers
Around 1 pound of small plastic/mylar strips that come off the side of a flat screen TV "screens", which have gold fingers incased in plastic or glue) After incinerating, the strips weighed ~22g

After filtering the jar with AP in it, the total material from both jars combined was ~7.8g

I put the wet filter with the powder/material into a melting dish. There was a little plastic/glue left in it.

I added some borax, then began to re-incinerate, but ran out of fluid about halfway through. Some of it barely melted and I know some of the coffee filter was still in there "burnt".

I don't know why, but I decided to try and dissolve the material with HCl/Cl.

Made a fresh batch of stannous, and tested the solution. Negative. Added a couple more mls of Cl over the next couple hours. Still negative. The solution was VERY dark green. Total amount was approx 20ml HCL, 30ml CL.
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I came back the next day and tested the solution. Negative. I'm guessing there was alot of copper etc., still in it and a possibly a tiny bit of iron, which pushed out any gold.

I filtered the material and put the negative solution into my stockpot, just incase there actually "was" anything in it.

I used a separate beaker for the powder/material. Not sure of the weight for this, which now also has some burnt filter in it.
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Day 3, I tried HCl/Cl again, slightly lighter green solution. Stannous positive for gold finally. I filtered the solution, rinsed it down and tested it again. Negative. :?: Ok, I must have diluted it too much.

Approx 50ml HCl, 50ml Cl and ~60ml tap water. Total solution ~160ml.
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Day 4 (today) Tested negative. I figured I would try to drop the material out, to see if I did have any gold that was getting a "false positive" from iron etc.

I put sand on my hotplate, to evaporate the solution from 160ml to ~75ml, to remove the CL so the SMB works. (Hotplate with sand worked really well)

Stannous showed positive again. It looked extremely black, so I let it sit there for about 10 minutes and rinsed it off. Nice purple stain :p

After the solution cooled back down, I took SMB and added maybe a gram or 2. (I'm guessing there was around 3-4g of gold in the material)

Tested with stannous, positive. Added another couple grams of SMB, still positive, a couple more... STILL positive :?:

I continued to get a positive for stannous "purple/black on paper towel and on spot plate", even AFTER the SMB stopped giving a reaction "I added about 1 gram after that also". There was a strong sulfur smell coming from the solution. (the smell burns the eyes and nose a bit if anyone was wondering, actually made me sneeze, so I went out into the yard for a few minutes).

Total SMB used was between 12-15g.

I've been thinking, that since the solution was ~160ml, and ~50ml of it was Cl, when I evaporated it to 75ml, if all of the tap water evaporated, there could still be up to 25ml of CL in it, which might be why it took so much SMB, and still shows positive for gold. Unless it's a false positive.

I gave it about 5 minutes and checked with stannous again. still positive, but this time when I used stannous , it also made an oily blue/black "grease?", that stays on top. (I have no idea what this is, possibly micro pieces of the burnt coffee filter floating on top?)

The solution is now orange-red and theres a light brown/yellow precipitate at the bottom. Looks almost like the clean gold powder precipitate in other threads.

I couldn't possibly have THAT much gold in there could I?, It has to be iron or something also? (I highly doubt there would be any PD or PL in it) There is about 1 inch of solution in the beaker and 1/2 inch of it is the brown/yellow precipitate.

I only let it settle for a few minutes, when I saw that mass of brown/yellow precipitate, so I may be mistaken on the amount. It looked like a lot.

I'm letting the solution settle for a day. There is probably alot of salt at the bottom mixed in with any gold that dropped making it look like more, since it may have been completely neutralized from adding SMB until it stopped reacting. "Even though the solution still shows positive for gold"

Anyone have any ideas?

I'm thinking about evaporating it dry and starting over with fresh AP.

The left over material, that was in the 3 filters, still has un-dissolved pieces of metal in it, which looks like alot of previously burnt filter paper "powder" and tiny gold copper flakes.

Once I get more fluid for my torch, I may just melt everything and start over. I'm going for 999 :mrgreen:
OK, so, would you believe that I had the exact thing happen to me and I did almost the exact things you did and the outcome was almost the exact. I DID however take pictures and videos. I'm going to attach a picture of my solution after I put some on my spoon for testing..I'm hoping I will be able to attach it. I'm pretty sure we both dropped PD..
 

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OK, so, would you believe that I had the exact thing happen to me and I did almost the exact things you did and the outcome was almost the exact. I DID however take pictures and videos. I'm going to attach a picture of my solution after I put some on my spoon for testing..I'm hoping I will be able to attach it. I'm pretty sure we both dropped PD..
Welcome to your second post!

Why do you think you have Pd in your solution?
Your stannous seem to be a false positive aka Copper or SO2 positive.

You did not get a proper welcome when you arrived of two reasons.
One, your first post did not sit well:
https://goldrefiningforum.com/threads/gold-precipitation.26910/post-367010
Next, there was no refining indicated in that post, now that you have obviously ventured into refining
and on top of that even PGM refining we can not wait any longer.

STOP now, we have members who have died of PGM related exposure.
Put your stuff/toys away a safe place and study.
When you think you have the hang of it present a plan and we will comment on if it is a sound approach or not.

Here for your studies:
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/
 
OK, so, would you believe that I had the exact thing happen to me and I did almost the exact things you did and the outcome was almost the exact. I DID however take pictures and videos. I'm going to attach a picture of my solution after I put some on my spoon for testing..I'm hoping I will be able to attach it. I'm pretty sure we both dropped PD..
Can you please describe in detail what you did?
Step by step, too much wrong with what Grelko did so I hope you did not copy him.
 
Can you please describe in detail what you did?
Step by step, too much wrong with what Grelko did so I hope you did not copy him.
No no. I did that a.while back before I started dropping gold daily. I do a LOT of experimenting all day. I'm always bored these days as my significant other passed away in September so it's all I do now. When she was alive, I only messed around a few hours a day here and there, is around the time last year that I got that solution.. now I have other wild and mysterious solutions like the one I am about to post with questions.
 

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