Gold powder purification

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Rmwatson78

Well-known member
Joined
Feb 2, 2016
Messages
63
Location
Tucson, Arizona
Ok so I took all of my gold powder from various extractions since I started and boiled them in a hot nitric acid solution for about four hours until I no longer saw any colored smoke and it was clear that the nitric was either spent or exhausted from the solution. I then rinsed the 3000 ml of remaining solution with 5 gallons of distilled water and dryed the powder out once more. Then I placed the dry powder in a 5000 ml Erlenmeyer flask and added a 15 percent solution of hydrochloric acid and boiled for five hours or so until I could tell the solution was extremely thick. I washed the solution with another five gallons of distilled water and I'm now drying out the powder once more.

Does anyone have any tips on speeding up the process when it comes to drying out your gold powder?
When the powder is completely dry and placed in a smelting kiln how much weight will I lose when it melts if any?
I read somewhere that someone said to mix the dry gold powder I have with an equal amount of borax...is that right?
Thanks
 
No longer seeing nitric fumes doesn't necessarily mean the nitric is gone. Probably just means the nitric had dissolved all it would.

Did you incinerate the powders after the first drying? If not you made some AR when you added the HCl most likely. Check that second 'rinse' with stannous. Sounds like you may have missed some values.

If you didn't incinrate any chloride out of these powders before the nitric, you may want to check that first rinse also.

Did you mix 5 gallons of water with each solution then filter? Or did you filter then rinse?
 
I'd suggest testing all the solutions if you didn't incinerate before each step as there may be values in all of them.
When I was refining full time a used a cheap plug in oven and simply washed the rinsed powder into a clean Pyrex dish or plate and placed it in the oven, it's not very fast but it doesn't need watching.
 
Sure there are ways to make this process both more efficient and quicker. Could you answer Goran's very valid question here as it will clarify a few things. My initial observation would be that both the volume of liquid being used appears to be excessive, and the process you are using appears to be flawed, but your answer as to gold quantity will honestly help us to help you.

Jon
 
Hehe, sorry Jason!

Just worried he is going to toss a good amount of Au with the 10-20 gallons of gold bearing waste he's already created.

If nothing else, I do sincerely hope you are being safe with all of this Rmwatson.

Ben
 
The resultant powders I have are from the incomplete processing of 75 lbs of gold plated cable connectors, 12 ounces of ram gold fingers, 750 grams of gold plated materials of varying type processed in a sulfuric acid cell, and approximately 12,000 grams of various lots of gold filled jewelry. My math on the approximate ball park gold content of everything is more than just a few ounces, but I'm definitely not speaking from experience.
 

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Are you still getting the same melt result after all that leaching?

Have you tested your waste solution with stannous?

With that much material you should definitely have a fair amount of gold somewhere! 8)
 
You have quite a mix of materials there. All I'm reading about is your powders. If you have not anywhere along the line put your gold into solution, then filtered, then selectively precipitated gold, then whatever solids you have are going to be a very mixed bag. No matter how much rinsing and boiling you do, you would still need to get your gold into solution, filter, and precipitate before you can expect a decent looking melt.

Perhaps I'm assuming too much. But have you dissolved and then precipitated your gold at any point?
 
Your melt looks more like a piece of copper oxide slag. Hit it with a hammer, slag crushes while gold flattens out. Just don't loose any pieces, though it looks like a glass it could have fine grained gold powder in it.

Are you able to melt a silver coin of similar size? It might be that you don't reach high enough temperature to melt the gold so it only mixes with your borax and creates a glass with powder suspended in it.

You should do some tests on smaller amounts of material before going on to a bigger lot like this. I suggest that you stop experimenting with the big lot and concentrate on smaller lots. Last week I refined the gold from one gold finger (4 gram of circuit boards). I worked in test tubes and with drops of acid and it worked just fine. The only thing I have left is to melt the gold into a microscopic button, then I will make a post about it.

What I recommend you to do is to stop all experimenting. Then read up on making stannous and a small amount of gold standard solution. The gold from a single finger is enough for the standard solution, pale yellow gold chloride is easily detected. And then test the solution with stannous so you learn how a positive gold test looks like. Then star testing all your solutions to see where the gold is.
It may take some time, but your gold is still there somewhere as long as you don't throw anything away.

Solids can be tested by taking a small sample, then dissolve all metal and test the resulting solution.

This is not a complete instruction on how to recover your gold, you should keep on studying a lot before going back to the large lot.

I'm quite sure that the gold is not where you think it is.

Göran
 
Hi my friends!
I've never worked with such a dilute solution. Does cementing all the values on copper work effectively and will they settle out properly under those conditions?
I'm thinking that he may be better off to cement, recover the powders and start over after some studying.
artart47.
 
g_axelsson said:
Your melt looks more like a piece of copper oxide slag. Hit it with a hammer, slag crushes while gold flattens out. Just don't loose any pieces, though it looks like a glass it could have fine grained gold powder in it.

Are you able to melt a silver coin of similar size? It might be that you don't reach high enough temperature to melt the gold so it only mixes with your borax and creates a glass with powder suspended in it.

You should do some tests on smaller amounts of material before going on to a bigger lot like this. I suggest that you stop experimenting with the big lot and concentrate on smaller lots. Last week I refined the gold from one gold finger (4 gram of circuit boards). I worked in test tubes and with drops of acid and it worked just fine. The only thing I have left is to melt the gold into a microscopic button, then I will make a post about it.

What I recommend you to do is to stop all experimenting. Then read up on making stannous and a small amount of gold standard solution. The gold from a single finger is enough for the standard solution, pale yellow gold chloride is easily detected. And then test the solution with stannous so you learn how a positive gold test looks like. Then star testing all your solutions to see where the gold is.
It may take some time, but your gold is still there somewhere as long as you don't throw anything away.

Solids can be tested by taking a small sample, then dissolve all metal and test the resulting solution.

This is not a complete instruction on how to recover your gold, you should keep on studying a lot before going back to the large lot.

I'm quite sure that the gold is not where you think it is.

Göran

I would love to read that post about making a microscopic button from one gold finger. I'm not sure if you mean one finger contact or one strip of finger contacts. Either way, I think that information and experiment would help a lot of people (myself included) learn the process without ending up with gallons of waste.

Most of my own experiments with this were very small scale refining. I did end up with a couple tiny pieces of impure gold extracted from various sources. I think they are in a little cardboard coin holder as a keepsake somewhere. The tiny scale experiments were enough to convince me that I need an actual lab with fume hood and scrubbers before doing any larger scale experiments.

Actually, the main reason I have been inactive in this hobby for years now, is that my small scale experiments showed me that I would need a lot more gold containing scrap than what I have.

As I said, I'm very interested in small or even micro scale versions of the processes needed to separate and refine the precious metals from the other scrap materials. It would be great if it you could continue on after the gold is captured and purified, and show the steps needed (still on a small scale) to get the other metals out of solution either in a usable or saleable form or as waste.

Geo's post and video about Removing copper from spent AP solution http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=52&t=23645 made me a lot more interested in this hobby. I was a little disappointed to learn that "It is chunky when wet but crumbles to dust when it dries." but it still looked nice. I still only have limited gold containing scrap so a small scale tutorial sounds great. I'm tempted to try to make that tutorial myself but your version would likely need fewer corrections than mine. I assume you would include the stannous chloride testing. I'd be tempted to try making my own stannous test solution using a mL or two of HCl and some solder salvaged off of the scrap circuit board.

Of course, I'm also tempted to make my own HCl from scrap PCV pipe and my own bleach from salt water and electricity so you might not want to listen to me. I know the cost would likely end up being many times more than the value of any metals recovered and the needed chemicals are still fairly easy to obtain (muriatic acid, household bleach, etc.) so this would be mainly an educational process. I do think it would be fun, especially if you ended up with even a tiny speck of gold in the end. Making as many of the needed chemicals as possible would just add to the fun. I have spent many hours and days panning, sluicing, drywashing, and dredging around looking for a tiny speck of gold before so I know a visible (even with a magnifying glass) piece of gold would put a smile on my face.

Sharing my own experiments (if I really do them) might not be the best idea. A little knowledge could be a bad thing. Let's see ... If I put some plastic pipe shavings into a test tube and heat it up ... Cough, cough ....

Please do share your experiments.
 
Thanks to everyone who replied. I have been using stannous chloride throughout and although I still have a number of solutions with an emerald, almost neon green like color testing positive for gold....I also have a rather large amount of "mud" that is non reactive to nitric acid or hcl by themselves, but definitely reactive to both when combined. I received 4 liters of Methyl Isobutyl Ketone I ordered yesterday in the mail to help me finish because I was unable to find Butyl Diglyme in sufficient quantity to treat all my materials. I'm hoping that the latest boiling rinse of the powder I have with HCL and a few drops of sulfuric acid will have removed the remaining base metals. I will now redissolve what I have in an A/R solution and attempt a solvent extraction using MIBK and oxalic acid.
 
bmgold2 said:
I would love to read that post about making a microscopic button from one gold finger. I'm not sure if you mean one finger contact or one strip of finger contacts. Either way, I think that information and experiment would help a lot of people (myself included) learn the process without ending up with gallons of waste.
One strip (4 gram) of circuit board. I was sent a power module from a mainframe and it had gold plate on the edge. I broke it off and did all the steps to refine it... actually I skipped the stannous testing as that would have been a relative large loss and the left overs ended up in the stock pot for sedimentation and recovery of any values left. I use stannous when I'm not sure what's in a solution or on any solution before classifying it as waste.

What is left is to melt the resulting gold and see if I could make another milli button. After I've melted it I'll make a thread about it, but I'm a bit limited in time right now. Too much work and Easter is coming up fast.

My previous small scale refining... gold from one IC. http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=7056

Göran
 
Watson... Can I call you Watson? I just like the name. This is just the opinion of one of the new ones here, and if you are being helped behind the scenes by one of the pros and if they are comfortable with it then I think that's great. Good luck with it.

But, while I am quite interested in solvent extraction and even processes that are even more involved, I find it wise to learn the basics first. I will get to those procedures later. I feel you may be making things more complicated than that need to be. Why not recover values from those waste solutions with copper, basic process. Collect all powders and incinerate, basic process.

Then on to a normal refine. Dissolve with solvent of choice. Eliminate oxidizer. Filter well. Recover with precipitant of choice. Wash well. Repeat if necessary. I know, oversimplified, but just trying to form a point as dull as it may be.

Granted that I have only done those basic, normal procedures a handful of times, with much less volume of material, it has given me the knowledge and confidence to build on to be able to move on to new procedures.

Anywho, just be safe and good luck.

Ben
 
Ok, so after incinerating my powders, i redissolved in a 1 liter 3to1 A/R solution and heated it to a slow boil for an hour or so until I could see all powders were dissolved and I let the solution cool overnight. I then added 500 ml of methyl isobutyl ketone to the A/R solution after transferring it to a half gallon mason jar. I shook the contents vigorously, pausing to allow pressure to release by unscrewing the lid and repeating about 10 times. I used a 2000 ml separation funnel to separate the organic solvent layer, and placed this layer in a 1000 ml erlenmeyer flask. I washed the layer with a 5n HCL solution and separated it again. I then made a 500ML 40% concentrated solution of H2SO4 and added it to the organic layer in an attempt to convert the chlorolauric acid solution to gold hydroxide, but I immediately got a reaction in which my almost clear yellow organic layer dropped a large amount of goldfish brown solid material to the bottom until it seemed that every bit of the H2SO4 mixture had been solidified at the bottom of the two layers as a shiny medium brown mass. It was actually quite a sight to see and I wish I had recorded it. According to my research, I'm now supposed to convert the gold hydroxide solution back to chloroauric acid by adding A 5n HCL solution to the aqueous layer but before I move further I want to know why it appears as if the gold has already appeared before getting to the next few steps in which I'm supposed to reduce with sodium sulphide?
 
As a relative newbie to recovery and refining, no insult intended, as has been stated before your going too fast and missing important steps.
After incinerating your powders, the reason to do so is to oxidise any base metals, you should have then used HCl over heat to clean your powders, the one good reason to do this is it removes tin plus many other base metals making for a cleaner final solution, once the material has ceased to react decant and plenty of hot water rinses and then go to the method of dissolution of your choice, filter as usual dilute and then perhaps use a different precipitant, the reason for that point is that precipitants can cause drag down of base metals but each will react slightly differently as to which they favour.
This process is well discussed and documented here on the forum and used by nearly all the members who regularly refine by going to solvent extraction you are limiting those who can or will help, even the chemists here will tell you that theoretical chemistry is or can be very different from practical chemistry when your working with volumes of materials and complex mixes of chemicals ,gases and environmental conditions.
Experimentation is a fine thing once you fully understand the basics, were it me I would have taken say 5 grams and tried out this process to see how and if it will work before putting all my hard won gold into an untried and new process.
You made mention of grumpy members well they have been here some time and have seen and heard all this countless times or variations of the same, you need to slow down and study rushing headlong into recovery and refining can be an expensive lesson in why we try to calm new members down.
We don't want you to fail or give up in frustration but in honesty reading and studying is the only option to avoid that, instead of chemicals in your hands you should have Hoke and access to the forum to check on points that make little sense, then baby steps using trial amounts and studying the reactions.
You can do this your obviously intelligent, if you take the advice as its meant you will look back in 6-12 months and cringe as what seems strange reactions or outcomes now will be expected and understood.
Good luck and get reading.
 

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