Help! New to forum! Have media from plating operation

[Absolutsecurity]

I had some soaking in hybrid nitric and it was a white yellow gunky mess as I stated before - I poured of the mess to wait to figure it out later and washed the balls and added straight lab grade nitric (my last stock) and it reacted well with red fumes - I ended up with a flask full of gold balls and dark blue/green acid solution with salt crystal looking percipitate (SILVER?) (as shown in pics) so I removed the balls with a maganet and left the percipitate and blue/green acid for a later date when I know what to do with it.
Some of the sliver balls totally stripped and are shiney silver/white metal (as shown in pics)

All the balls are magnetic - some are a little blackened and silver and the little cup contains all of them the black pan has the gold balls that look like with some new acid will go the same as the sivler ones!

HUMMMMM! They used these balls in all the plating - gold - silve - nickel and copper - SOOOO I am dealing with 5 metals here! HMMMM!

G

 

[goldsilverpro]

You'll never know whether the balls are non-magnetic 300 SS until you get all the nickel off one of them. Pure nickel plating is very strongly attracted to a magnet. Try vise grips and strongly squeeze one of the balls. Maybe, you can get enough pressure on a ball to break the plating enough to expose all layers. Then, use the hot nitric. I know that you can't do this in production, but, at least, you may find out what the core is.

Most of the common 400 series SS's aren't attacked with nitric that is at least 50%, by volume. Some, like 409, are more likely to be attacked.



I Just thought of a possibility. Mix up a small batch of the following recipe and run a couple of fresh balls in it. You may, or may not, need heat. Try it without heat first. Without heat, I think it will dissolve the gold, Cu, and Ni, without eating any type of stainless. It may take a day or two at room temp, but that's alright. Silver may prevent the dissolving, especially if it's layers are too thick.

All parts are by volume:

50 parts nitric acid
5 parts hydrochloric or muriatic acid
45 parts tap water

I have processed 1000's of ozs of gold with this solution. The problem with this is the large amount of nitric to get rid of before you can drop the gold. However, I have discovered that elimination of the nitric is totally unnecessary if you use mono hydrazine sulfate (lets call it MHS) to drop the gold. You just sprinkle the powder in, then stir, and the gold drops. Doesn't take much. The reaction is very stoichiometric (100% efficient) when reacting with the gold.

MHS is somewhat carcinogenic and a mask should be worn. However, it is shipped slightly moist to prevent dusting. The moisture causes clumps which must be broken up. I used to break them up by mashing them with the bottom of a 100ml beaker, in a flat-bottomed dish. I think a blender would work great. We need a MSDS for this chemical. Lots of things are carcinogenic. I had a good feeling that, if common sense and basic safety precautions are used, this chemical is pretty safe to work with. I would use gloves, a mask, and a fume hood or good exhaust.

Some of the pro refiners use MHS for the Pt Gp, also. I haven't tried this, but I seem to remember that it requires some pH control. I think I also remember seeing patents on it.

It seems you have quite a bit of money there. We'll eventually get you going, if you keep detailing, to us, what you've done and what the results are.

 

[Lou]

Hydrazine sulfate works terribly well for reducing almost anything, cleanly as well. Sulfate and nitrogen are the products. Much, much safer than straight up hydrazine.

I use it for the PGMs.

 

[Absolutsecurity]

AS GSP asked

I took some hybrid nitric I had sitting in a flask and added water and a few droppers full of HCL and the nickel balls - it took off like crazy - I got my teflon stirrer extractor and pulled the balls out and took this picture - they are down to the base ball metal and are rusty and still magnetic.

What does this tell us??

Im screwed because they arent hi grade stainless RIGHT!

This isnt gonna be easy huh!!?????

G

 

[Lou]

Well as long as you can get all the gold off without wasting too much nitric acid, you should be just fine. You'll have to re-refine the gold another time through. First time you'll get gold, but other stuff will co precipitate. Harold posted an excellent washing procedure to get rid of most base metals.


After I had the crude gold powder, I'd rinse water, then boil with nitric, remove from that, rinse again, give it rinse of HCl, then finally ammonia, and the another rinse with water. After that, dissolve it all over again in aqua regia or AP, and precipitate with whatever you like.



You have any sort of yield on these guys yet?


Edited.

 

[Absolutsecurity]

No yield yet - just did a small batch of the silver coated balls to see what thaey are before any plating was done. I have noted that I disolved 400g's of silver balls and I will see what come out of that and post it - I also have 200g's of gold rice shaped media sitting in nitric right now and the gold plating is slowly coming off them. When I can get back outside I will fire up the hotplate and see if some heat helps out again!

Glynn

 

[Harold_V]

After I had the crude gold powder, I'd rinse water, then boil with nitric, remove from that, rinse again, give it a nitric HCl, then finally ammonia, and the another rinse with water. After that,, dissolve it all over again in aqua regia or AP, and precipitate with whatever you like.

That's a bit confusing, or perhaps I didn't quite grasp your point. As I interpret the comment, you suggest a wash with nitric/HCl, which would simply dissolve the gold.

I never washed with nitric, and don't recommend anyone do so. It's fine before gold has been dissolved, but once you've precipitated the gold, even if the intention is to process it a second time, I always suggest one avoid using nitric until such time that you actually re-dissolve the gold.

My rationale, for what it's worth, is that it's almost impossible to remove all traces of chlorides from the precipitated gold, so you end up re-dissolving some of the gold when your intention is simply to wash it.

I suggest a wash in HCl and water, a rinse in water, a wash in ammonium hydroxide, a rinse in water, a wash in more HCl, and a final rinse in water. That way you don't risk re-dissolving any of the gold until you're ready to do so.

All of my washes and rinses are taken to the state of boiling, and allowed to work until I see no changes in the solution. I found that each batch had different requirements, depending on the nature of the precipitated gold, and the level of contaminants that were present.

Harold

 

[aflacglobal]

They look like Civil War musket balls now.

 

[Absolutsecurity]

I wasnt even trying to recover values - I was just trying to get to the center of the tootsie pop!!!!! LOL!!!!!

If you look at my distilled post you can see the gold flakes that I filter off to work later when I have more as well as the silver that I cemented out!

This was just a batch of silver balls (I have 50+ more #'s ) I have the gold balls (40 + #'s) to work but everyone wanted to know whats in the center -0 so thats what I was trying to do!

I want to thank everyone for helping me! I am keeping track of what you guys say - and its working! :wink:

THANK YOU!

Glynn

 

[Harold_V]

What does this tell us??

One thing it tells me is that you may not be seeing rust, but cemented gold. If the balls came out as they appear, that's probably not rust. If, on the other hand, they were not rusted until after they were washed, I'm wrong.

Here's the problem with base metals. As you dissolve the values, acid is consumed. When the acid level isn't high enough to continue dissolving the values, the base metal starts precipitating the values. In the process, the base metal(s) go in to solution, and the values are converted to a solid. Although gold appears to your eye as a shiny yellow metal, that isn't necessarily true of precipitated gold. It commonly precipitates as finely divided particles, which do not reflect light in the same way that a solid piece does. The result can be anything from a light tan to an almost black precipitate. The color on the balls very much reminds me of such a precipitate. You might test a few by vigorously rubbing to see if it wipes off, or shifts to the more familiar color of gold.

Assuming they are iron (steel), and assuming they are doing what I suggest, all is not lost. They can still be processed by acid, but you'd have to be smart in how you'd handle them. One way would be to dissolve the entire mess, then selectively precipitate the values, with the idea in mind that you'd have to re-process the gold due to heavy contamination from drag down.

Harold

 

[goldsilverpro]

AS,

What do you mean by "hybrid" nitric? Nitric made with a nitrate and sulfuric? If so, we've been talking apples and oranges.

If you are using "real" nitric, repeat the 50/5/45, HNO3/HCl/H2O experiment again. But, MEASURE!! the chemicals this time. I would also try 2% HCl, instead of 5%.

I'd still like to see what happens, on one ball, with aqua regia made with "real" nitric. Except for silver, it should dissolve everything. You may have to ultimately do this, if all else fails. If you do, I'm thinking you can drop out the gold with a copper buss bar. Copper not only works on silver, it also works on gold and the PGM's.

Most every brain on the forum is trying to help you do this. Like I said, this type stuff is extremely complicated to dissolve.

I hope every member reads this thread and I hope more join in. It's terribly instructive because it gets to the core of what experimentation, practical dissolving, and the chemistry, are all about.

 

[lazersteve]

Glynn,

I just home from work and your samples have arrived (WOW that was fast!).

I started off by melting a single gold BB with my torch (about 10 seconds to melt; it produced lots of sparks) and then tossed it in some plain Jane muriatic acid (31.45%). After a little heat was applied the reaction kicked in (3 minutes heat time) and the iron core is now dissolving rapidly.

Once the core is gone I'll take the residue up with some HCl-Cl and see what comes out.

This is my first idea , despite the fact that it may be impractical with the quantitiy of these BB's that you have. It definitely seems to be working with HCl.

I'll try a few more experiments with some other ideas to see which is best. I really like GSPs approach.

Steve

 

[Absolutsecurity]

Hey Steve,

I sent them priority mail! LOL!!

Did you get my post and PM on the other post? Im worried - I watch your video and I thought if I used nitric on the silver balls and used copper to cement I wouldnt have and chlorides just silver metal - PLEASE TELL ME IM NOT WRONG PLEASE!!



Hey GSP,

I just got some more nitric 70% - so I will try again with one ball with the measured way you say - whats wrong with the hybrid nitric? I used con sulfuric drain cleaner and sodium nitrate dry and had it sitting soaking for a week before I poured off to use it. ( its not real nitric huh?)

Glynn

 

[lazersteve]

Glynn,

I posted a reply to both your PM and the other post. If you used copper to drop the silver you are good to go, it just looks very white in the photo (like silver chloride).

The 'hybrid' nitric is real, if you kept it below 0 C for over a week you definitely have some quality nitric. The reason GSP has concerns is due to salts which may not fully convert in the 'hybrid' method if you rushed the reaction. If you follow my directions to the letter you will have next to no salts dissolved in the 'hybrid' nitric. Another source of impurities in the 'hybrid' nitric are buffers and junk from drain openers (dark black colored) if they are used instead of the concentrated battery acid (clear).

Steve

 

[Absolutsecurity]

MAKIN MEATBALLS I'LL BE BACK! LOL!

G

 

[Platdigger]

Steve, about the 'hybrid' nitric, what about any chlorides or iodines that may be in the sodium nitrate?
Randy

 

[Lou]

If there are halides present, you will see a precipitate if there is silver or lead in solution. A good analytical test for lead and silver is the formation of their highly insoluble iodides. Even very dilute lead solutions will produce a yellow iodide precipitate.

So if your nitric is contaminated, you will have a hazy solution, and it will work less effectively. The only ways around this problem are to a.) distill the nitric acid, b.) use a reagent grade nitrate salt that is halide free. Remember to use distilled water.


Edit: I was thinking, if he can get ahold of some KCN, that would be a very good method to strip off the gold cleanly and quickly.

 

[Absolutsecurity]

Hey GSP I did that 50 45 2 deal and the ball started fizzing and then got coated with white fuzz and I broke some off and it keep getting fuzzed up again - I pulled the ball out and there was a gold coating under the white fuzz - I chipped some of the white fuzz off and have a half rusty ball and gold - see pics..

G

 

[Absolutsecurity]

Your gonna like the rice grain gold pieces I sent you - had som soaking in nitric for 4 -5 days and put it on the hotplate tonight - gold flakes galore!!

G

 

[aflacglobal]

This is a good thread.