Gold Nugget not dissolving

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Noxx

Well-known member
Joined
Feb 24, 2007
Messages
3,365
Location
Quebec, Canada
Hello,
I've puted two gold nuggets in Aqua Regia. One dissolved completly but the other one turned black and did not dissolved... Why ? Is it because there is silver preventing it to dissolve ?
Thanks
 
Noxx,

It's some sort of impurity, could be flux, higher PGMs, or silver chloride. Silver chloride is usually white though. Does heating the solution cause it to dissolve?

Steve
 
If you have the ability noxx---it's best to roll your nugget out or flatten it.

Heat it up a tad and roll it or pound it flat. Twist it so it doesn't lay flat in the dish. The more surface area for the acid to work the better.

You may not have had enough AR to complete both nuggetts too.

I've had the same happen with electrical contacts. So I just digest one contact at a time.

Hope that helps.

AgAuPtRh
 
OK, I just took my nugget from the acid mixture... My nugget isn't black. It is has a deep purple layer (easily removable). What is it ?
Thanks
 
Well, it's not... It a kind of wax. As soon as I puted the flame on the purple powder, it melted instantly into a ball. When cold, this bullet is hard rock lol.
I don't know what it is...
 
The action of hydrochloric acid on silver--even in aqua regia will turn the silver a gray color developing a whitish layer of silver chloride. It can turn purple in sun light.--a lavender color then turn to black.

After heating your nuggets in aqua regia---what color did the solution turn to?

Karat gold---gold alloy with copper will turn green.
 
It was mostly pure gold nuggets +95%. My solution took a yellow color. But it was outside so sunlight may had an effect.
Thanks
 
Heat it up a tad and roll it or pound it flat.

It is likely hot short, thus won't respond to heating---it will simply crumble if so. Pounding on it would result in lost alloy. Gold is not known for being worked hot with success. It should be rolled cold----or melted and poured in water to create "corn flakes". They break down readily, assuming silver content isn't too high. If they are, the button should be inquarted, pelletized (corn flakes), then base metals removed with nitric acid before attempting to dissolve the gold with AR. It's never a good idea to attempt to process buttons of metal. It takes too long.

You may not have had enough AR to complete both nuggetts too.

Highly unlikely. Both would have been dissolved somewhat equally were they of equal composition. The problem is likely a presence of too much silver, or an insoluble element, though how that would have been combined with gold I have no clue.

If the button had a green cast before beginning the operation, most assuredly the gold contains too much silver. While silver chloride is white, it isn't when it doesn't form freely, such as when precipitated from a nitrate solution. When one attempts to dissolve gold in heated aqua regia that contains too much silver, it will eventually have a dull, green cast, and will resist dissolving indefinitely. You can boil it for days on end with no results. The presence of silver, reacting with chlorine, creates an impervious shell of silver chloride which isolates the gold from the acid. It is that shell that appears to be a dusty green color.

Harold
 
Yup noxx----even reagent grade acids can be limited in how they work. Giving the acid as much surface area as possible by rolling and flattening can increase the acids ability to work and also help the acid to work faster.

The build up--waxy stuff as you put it--if it turned color after coming out of the acid--was probably silver and probably the reason your nugget stopped digesting.

Sun light shouldn't have an effect until your chlorides are out of the acid and shouldn't effect the color of the acid at all.

Digesting all of the base metals first----before refining your gold will help you refine a purer product. So---if you do a hydrochloric acid first--wash--then do a nitric acid---wash---then you are left with as much gold as possible before treating with aqua regia. By removing the base metals first you also have less garbage for the acid to work on and less garbage in the solution from which you will be dropping your gold.

Roll and flatten
Treat with hot hydrochloric
Treat with hot nitric
Wash between treatments
Finish with Aqua regia

A purer gold will result.

Patience is the key
 
AgAuPtRh said:
Roll and flatten
Treat with hot hydrochloric
Treat with hot nitric
Wash between treatments
Finish with Aqua regia

Sigh!

Your sequence is wrong. Once you introduce HCL, you can't introduce nitric, and if you introduce HCL first, you won't remove silver.

Nitric should be the first reaction, removing all base metals. If the gold is properly inquarted, there will be very little base metal and silver left in the now honeycombed gold, and won't present a problem. Washing the lot one time with tap water is adequate, then AR should be introduced. What little silver is left behind will readily convert to silver chloride and be recovered when the gold chloride solution is filtered.

As an added note, nothing to do with this particular post------there is absolutely no need to use distilled water in any of these processes. A small amount of silver will convert to silver chloride, but that is not lost. Trace elements in tap water, aside from chlorine, present no problems for the refiner. There is no need to spend money for distilled water unless one is working with silver nitrate intended for use as an electrolyte, or making test or standard solutions.

Harold
 
Thanks for all the great info. I'm currently building a tutorial on the subject.
But note that my nuggets are +95% purity before I added them to the AR. Maybe the one who did not dissolved had a surface layer I don't know...
I will try to «corn flake» it lol :lol:
 
Noxx said:
Thanks for all the great info.

You're welcome!

I'm currently building a tutorial on the subject.

That's nice------but it would serve the readers very best if it was good and proper information. There are tried and proven methods for standard refining that are easily accomplished----with no real reason for anyone to "re-invent" the wheel. There's a fair amount of misinformation being tossed around that is sure to create problems for some of these guys, or complicate what should be an easy process. Working with silver chloride is one in particular.

I'd suggest you do your research well, and choose a procedure that is in keeping with good practice. Lots of wives tales need to be abandoned so these guys can move forward with proper learning.

But note that my nuggets are +95% purity before I added them to the AR.

I'm curious how you know that. Properly refined gold should exceed 95% first time through, and have almost no silver. Rose suggests that a few atoms of silver will behave as gold and be difficult to eliminate, so a trace, at best, should show in once refined gold. Other base metals may differ, but they wouldn't prevent the dissolution of gold in AR.

After posting my comments, I read further and agree, the purple film you found was likely silver chloride, but it had obviously photo-reacted with sunlight. It's also possible for the gold chloride, absorbed by the silver chloride, to have done the same thing. Gold chloride, exposed to light, will leave purple stains on almost anything it touches Everything you described typifies what you would have experienced had it been silver chloride. The green coloration I spoke of would have been only if you had been working out of sunlight, and had not photo-reacted.

I assumed you were working indoors, in a fume hood, ---but realize most of these guys don't have that luxury.

Maybe the one who did not dissolved had a surface layer I don't know...

I have serious reservations about a "surface layer", aside from one forming from residues that accumulate (like silver chloride).

I will try to «corn flake» it lol :lol:

They work great. By the time the insoluble layer has formed, the entire lot is usually dissolved, so the silver chloride just crumbles and turns white----and all the gold goes into solution. You may wish to look for some tiny bits that don't fully dissolve, for occasionally one of the flakes will have a heavy cross section. This process works very best if you use it for the preliminary operation, where you remove base metals via the inquartation/nitric process.

The process of making the corn flakes is simple. Have a deep container (metal----never plastic), at least the size of a 5 gallon bucket. A grease can, one you might see in a place like Jiffy-Lube (about 20 gallons in size) would work great, but should be well cleaned if used). Fill the container with cold water, then melt your button with a torch. Pour the molten metal into the water filled container in a thin stream, moving around the container so you don't get an accumulation of hot metal in one place. It can fuse to the container if you don't have enough depth, or poor too much in one place at one time.

You don't get shot when you perform this operation, you get, instead, flakes, best described as corn flakes, thus the name I applied.

If you need to talk about the inquartation process, ask. It's fairly critical, in order to get the base metals out without breaking down the gold into fine powder. Hoke's book covers it perfectly, which is one of the reasons I keep telling you guys to buy the book. It also teaches you how to test metals.

Harold
 
Harold,

I'm very interested in learning this process properly. I've come to realize, since meeting you, that there are much easier ways to do these things and you seem to have a very good grasp on what the CORRECT processes are. Please share your valuable knowledge with us.

I've begun accumulating some sterling silver items which I'll soon purify to elemental silver for use in these processes.

Thank you again,

Steve
 
Thanks for this very valuable info.
I'm currently learning how to inquartate properly. But I'm looking for a good place to get cheap silver ;) I don't have any at hand, I only have jewelry that is +14kt so Nitric Acid can't dissolve it...
Thank You
 
After going back and reading a bit--I see where I messed up in the process. The hydrochloric wouldn't help. That was from another testing process.

But I did find the next two paragraphs in C M Hoke's, Refining Precious Metal Wastes. It deals with "button" of melted Gold.

" If you have melted your filings into a button, the next step is to get the button in such a form that the acid can act readily. Sometimes it is so soft that you can roll it easily. Cut the rolled strips up short and twist them so that they will not lie flat in the acids. Roll them very thin; a few minutes at the rolls will save hours in later steps. Anneal.
Usually it is easier to granulate the button than to roll it. Remelt the button in a clean crucible with a little flux, and pour it while molten into a big bucket or tub of water. Pour it in a thin stream and the molten metal will break up into fine shots or pellets when it hits the water. Collect these pellets carefully."

Refining Precious Metal Wastes-C M Hoke 1940--pages 39 and 40.

This goes on to discuss the 'Nitric process" not hydrochloric.

Thanks Harold. I'm glad you are here and appreciate the professional experience you bring to the forum. I hope you stay around for a long time.
 
I tried to put it again in new Aqua Regia and it's still turning black ! My solution took a yellow color but the reaction seem to slow down. I already remelted the nugget and pouring it in water.
Here is what my nugget looks like after pouring it in water.
 

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Harold_V said:
Washing the lot one time with tap water is adequate- as an added note------there is absolutely no need to use distilled water in any of these processes. A small amount of silver will convert to silver chloride, but that is not lost. Trace elements in tap water, aside from chlorine, present no problems for the refiner. There is no need to spend money for distilled water unless one is working with silver nitrate intended for use as an electrolyte, or making test or standard solutions.

Harold

Harold, once again you surprise me.

Please indicate what scientific basis you are relying upon to support your statement which apparently exempts ANY chlorine present in tap water used by these forum members? Yes, chlorine as you note is most assuredly currently available in tapwater. I would add those amounts vary depending upon ones distance from the substation where Clorine is routinely added by municipal water department personnel.

Chlorine is one of the most potent of the 5 gold dissolving halogens. This is true when forum members are using sodium nitrate as well.

Can forum members assume you have some scientifically based quantitative measurement as to how much gold loss is acceptable, due to chlorine in tap water?

It appears all forum members agree water is the preferred diluting solution for their urea nitrate muriatic based solution.

Were you trying to say that because AR was about to be employed as the next step, that tap water wouldn't be any problem at this juncture with the exception of the chlorine in tap water?

How much gold loss is not acceptable to you? Or, should gold loss due to the exception you made for chlorine in your above quote be acceptable to others?

It looks to me like these forum participants are scrapping and scraping for every brown powdered particle they can possibly corral or capture in their filters.

Cost calculations versus results do not seem to be on high on their list of concerns.

a man named Sue
 
Noxx said:
Thanks for this very valuable info.
I'm currently learning how to inquartate properly. But I'm looking for a good place to get cheap silver ;) I don't have any at hand.

Have you investigated any metals besides silver for your inquart process?
Silver is not your only option, fortunately.

Since you are obviously into experimenting and reporting visually on outcomes, perhaps you would consider a series of videos showing various silver substitutes and how they perform in your process.

It should be an absolutely fascinating series. May we look forward to seeing some results of your experimental based research on this substitute for silver series in the near future?

a man named Sue.
 

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