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Butcher,
I have another problem. I had at least 1, maybe 2 large pieces of Platinum Jewelry that tested to be Platinum. These were large brooches so there was a good bit of Platinum in these pieces. I think my wife added them in my last refine when she helped me clean up (one) day. When I decanted the first couple of times my decant solution was black, not greenish blue but black. I have read on the forum that Harold says that Platinum will dissolve in Nitric if the solution has silver in it. I know I had silver in the solution and I feel sure that my large Platinum pieces went into this last batch I ran. I have tried to get the silver to drop out of solution but I can't get the silver to drop? I know I have silver in it but it will not drop. I put a couple of drops of this black solution into a little HCL. I did see a little white cloud like appear this time. The first time I didn't see it, but I did the steps again and watched more closely. I believe I have dissolved my Platinum pieces in this black solution as well. I don't know how to go about recovering my Platinum out of these black decants that I feel my Platinum is in as well as silver? I have about 6 gallons of this blackish solution? Nothing that I have read addresses this particular circumstance? Can you give me any help with this?
Thanks Butcher,
Oneal
 
If I understand you correctly this is a nitric acid solution used to dissolve the silver, but I would need more detail of conditions before this point to answer the question. Was this an alloy of gold and silver you in-quartered and shot that you believe you may have added platinum to by mistake, or what was the source and treatments prior to nitric acid?

Let’s look at some things while I wait for more detail.

Platinum will not dissolve in nitric acid.

Very little to no platinum will dissolve in cold aqua regia (a small amount fine platinum powder May somewhat).

Platinum is even difficult to dissolve in hot concentrated nitric acid but will go into solution slowly (powders would be somewhat faster).

If platinum is alloyed with (melted with) ten times its weight in silver then it can be dissolved into nitric acid.

So from the above your platinum would normally remain as powders if they were alloyed with gold and silver as quartered gold and silver, when being parted in the nitric acid solution, this would mean the gold powder (gold powders, also platinum powders mixed) which is insoluble in nitric acid would be left.

Lets look at the nitric solution for a second, unless you melted the platinum with a very high content of silver then it most likely contains no platinum, and you said you had a reaction (adding HCl of milky solution) indicating you still have silver in solution, which means to me, until you get all of the silver out of this solution (replaced by copper, or converted to insoluble silver chloride) you will not get the platinum out of solution if it is dissolved into solution, lets look at it as if we cemented out silver onto copper (too much free nitric acid may keep our silver dissolving back into solution until the copper nitrate uses it up, then silver will cement out first, if we did have platinum in solution it would cement using the copper buss bar after the silver was out of solution, this may be a very slow reaction, so it could take days. (It sounds like you still have silver but I am not convinced of platinum at this point).

Ok now thius solution of silver nitrate what if we had added NaCl table salt, or HCl to convert the silver in this silver nitrate solution to the insoluble white silver chloride, and what would happen to the platinum (if any was in solution), well some may be dragged down, but also we added HCl or chloride to this nitric solution so we now have made aqua regia, which would help to keep the platinum in this dilute solution, until we concentrated the solution and precipitated it with ammonium chloride or some other chemical reaction.

Now let see what would happen with our gold powders from above (for the sake of argument were mixed with platinum powders.

If we treated these gold and platinum powders, with cold aqua regia, platinum powders would not dissolve for the most part and would be left after gold was dissolved into solution as black platinum powders.
.
If we treated these gold and platinum powders in very hot aqua regia gold would go into solution first and then platinum would slowly dissolve also.

Lets say for sake of argument we had gold and platinum in this aqua regia solution, and we precipitated gold from a dilute solution after evaporation of free nitric acid, the platinum salts in this solution are water soluble, and would not precipitate using SO2 gas from SMB to precipitate the gold, if we did have platinum (after removing gold) in this solution we could concentrate it (to rid much water that platinum salts would re-dissolve in), and we could use ammonium chloride to precipitate the platinum.

We can also test solutions to see if we have platinum dissolved into solution.

There are several tests a person could perform on these solutions depending on what they were or what other metals may be involved in these solutions.

Aqua regia alone with platinum dissolved into solution the stannous chloride test.

Platinum with gold dissolved in aqua regia, a spot plate, precipitate gold with ferrous sulfate crystal, then move gold barren liquid to another clean spot in plate and test with stannous chloride.

The nitric solution I would cement out silver with copper buss bar (after removing silver) leave buss bar in solution and see if I did not get a black valuable cement from solution {possible platinum}.

I may also try to test this nitrate solution, in a spot plate some nitrate solution adding a few drops HCl, heat to evaporate and then test with stannous chloride, (other’s may have a better solution)


I have not worked with platinum, beside very small traces, I hope I will recover from my silver later, so my knowledge in this area is fuzzy, if someone see’s where I may be wrong, or if they can give Oneal better advice please speak up.

Oneal I hope you can follow my thinking, and please fill in some of the details needed here, so if your platinum did go into solution we can find it, but for some reason I do not think that it did, hope you keep stock pots, and your solutions (including waste)until you find it.

On second thought your platinum is probably the last place you left it, and the last place you will look for it. (Joking around), I hope you do find it soon.

Edit to add my thought on the melting dish, looks good, you have been doing something right, I will let Harold, give the advice on gold purity, as I am still learning too.
 
Oneal58 said:
I went back out and took a picture of the melting dish I have been using. I have melted 7 buttons in this dish. You tell me what you think?
The dish shows the characteristics of gold that is slightly contaminated. The color in the bottom, green/blue is typical. The pink/purple color around the rim is typical of colloidal gold that has been deposited in the melting process. It's not a bad sign, aside from the fact that traces of gold are lost from the melting process. Just traces, understand, and there's not much you can do about the minimal loss. The values will be recovered in due time, assuming you process discarded melting dishes.

Do I need to refine all the buttons again.
That's a judgment call, Oneal. If the gold goes to a refiner, it likely will get refined again, even if you do it twice yourself. If your buyer is an end user, I'd suggest re-refining, in particular if there's even a hint of a chance that your gold has traces of lead included. If it hammers well, without splitting, it's probably fine, though. Traces of lead make gold very brittle.

I looked closely at the buttons again and it looks as though 1 of them has a tint of purple on it. This one could very well be the culprit of what you are seeing in the image below.
If you find a trace of purple on your button, it's likely encased in a trace of flux. I don't recall ever finding purple on my gold, although if it's contaminated bad enough, the entire surface could be discolored. What to look for is a shiny surface, one that looks gold in color, and has no rainbow effect anywhere. I've already mentioned a deep pipe. Gold that is contaminated won't pull a pipe, so anyone that sees your gold that knows anything about gold will recognize the pipe as an indication of quality. The novice may not understand that, so don't be discouraged if someone makes a less than flattering comment about the presence of a pipe.

My advice here? If you hope to produce fine quality, yeah, refine it again. I did that with all my gold, and did it routinely for years. There was often no need, but by running it a second time, traces that are less than desirable are eliminated. I never claimed 4 nines gold, but I felt comfortable offering a guarantee of no less than industry standard quality (9995) because of the second refining. It served me well for years.

If, by chance, your objective is strictly to recover gold for resale, and your buyer is not an end user, refine once, melt, then sell. That will minimize the amount of work and offer the best possible profit. If you do your work well, eliminating base metals before dissolving values, and introducing traces of sulfuric to eliminate lead, then follow a good washing procedure, you should be able to come quite close to 9995 quality. Your melting dish will tell you if you aren't getting the job done, as will the surface condition of the button.

Here's one thing to remember when melting gold. In the pure state, it's perfectly tranquil. It will melt peacefully, with a yellow green luminescence, and a bright, shiny surface. If you see any type of oxide developing from the center of the button, moving towards the edge, where it is absorbed by the trace of flux in the dish, you'll know your gold isn't pure. The dirtier it is, the greater will be the oxide I speak of. You should be able to melt your gold without flux and have it remain bright and shiny if it's pure. That's assuming you use clean equipment, of course. Do not use anything that's dirty when handling pure gold.

Harold
 
Hi Butcher, I am just getting in and reading your post. By the way thank you for your post. I have read over this post a couple of times, I will read back over the post with a fresh mind tomorrow a couple of times. It's after 2:00A.M. here and I been going all day.
Butcher, this was the largest refine, by my standards that I had tried. This was almost 4 pounds of gold filled/Scrap Jewelry. Broke Hoke's rule, beginners start with too large of lots!
This was a Nitric refine, evporate down, add more nitric, and do again, time after time. This went on for a couple of days? I finally ran out of 70% Nitric and started making my own. Finally, I figured out something was wrong, (using too much nitric to dissolve this gold filled compared to other lots). What caused this I believe is that I let the solution evaporate too long 1 time. I had too many Irons in the fire at one time and lost track of time. Due to this I had a nearly 2" thick brick of what I will call a (metal salt brick) form on the bottom of the 1800ml beaker. The Nitric would only work on the outside edges of this brick. It (The Brick) had all the gold and all the undissolved metals locked up in it? The Nitric could not get to the metals to dissolve them but this brick would use up the Nitric but not getting any work done? I decanted, I had to break the beaker to get the brick out. I cut the brick apart with a large pair of side cutters and then crushed the pieces up with another set of large linemans pliers.
I finally got the Nitric back to doing the work it's suppose to. This is where the black decants came into play. The first 2 decants I had were black? Then they turned the common greenish color.
If I understand you correctly and please corrrect me if I am wrong but the first thing I need to do is check to see if in fact the platinum is even in the solutions.
1-I will use spot plate to test nitrate solution/add few drops HCL/heat to evaporate/then test with stannous chloride, if barren, do the following.
2-Aqua Regia solution with values, a spot plate, precipitate gold with ferrous sulfate crystal, then move gold barren liquid to another clean spot in plate and test with stannous chloride.
If no positives for Platinum shows up here, I can stop worrying and start looking where my wife put those Platinum Brooches. I might have to let her back in the house long enough to find them. :lol:
Butcher, it's got to be the last place my wife left it, she is getting blamed for it regardless of who misplaced the pieces. It's too late to beg off now if I am wrong, the damage is already done. :lol:
Let me know if I am going about this wrong Butcher, I am really tired tonight and very well could be off base.
Thank you for your post.
Oneal
 
Hi Harold, thank you for your post and directions.
Harold I believe I will get into the habbit of doing a re-refine on each button lot I produce. I have to melt it again anyway to get buttons into a bar so I think I will just go ahead and re-refine each button lot each time I have enough to pour a bar. I am not on production as you were in your business and can work on the lots I refine at leisure. But I am finding I spend more time on the refining than I did when I was working a job full time. I feel as you do though, the re-refining is not a bad habit to develope.
I have always followed your instructions on Making Gold Pure on every lot I have refined. I did not use any flux on any of the buttons I have refined. Reason was, when I was melting the buttons I did not see any foreign material or particulate on top of any of the buttons.
So, my decision is to just re-refine every lot I produce. If for nothing else but just self gratification and feeling good and confident about the lots I turn out. The Gold Filled Jewelry lots, dirty watch band tops, Etc;, have human skin, hair and oils on all the lots I refine. It is really rewarding to see what these beautiful pieces of gold were at one time and what they are now. It makes you feel really good inside. Hopefully without sounding arrogant, kind of proud of yourself.
I must note, without this forum and the free hearted individuals on this forum this would have been IMPOSSIBLE to accomplish on my own. And I must note also, especially one individual, who has been my tutor, just about every single day from the beginning, he knows who I am talking about.
Thank you Harold for your advice, This advice has aided me in making the right decision.
Oneal
 
Oneal


I would test solutions for the platinum.
If this broach was platinum I feel you would have noted it as something very hard to dissolve, if it did get put into solutions.

You could also check stock pot sediments, you would have to put some powders into solution most likely to test it,(as any metals higher in series would cement the Pt from solution in the stock pot).

Someone else may be able to give better advice, and have a better method to test the solutions.

If you did not melt the platinum with high volumes of silver, it would more than likely not be in the nitric solution, (no harm in testing, it would be better than my guess).

Oneal,
About the only thing I can give you advice on is, your wife is always right, I thought you have been married long enough to learn that by now. (I know I have been stubborn learning that lesson also).

It is much easier to re-refine the powders, (at final stage’s of the first refining process), before you melt them back into metals, (they go into solution with ease), this way it is not like doing a whole process over again, but is more like repeating final stages of the original process.

Also some suggest using a different precipitant the second time around.
Paying attention to Harold’s advice of trying to get out any lead that may have followed through the first refining, I would make a note of that, re-refining your gold will give you a chance to see how higher quality gold acts in solutions, and also it could show you how much impurity you may have missed the first round, although it does sound like you done a very good job with the first refining.
 
Hi Butcher, Thanks for your post.
I Acid tested the brooch and pendant probably 6 months ago. When I was just getting interested in refining.
First, I noticed that this material was much harder than any of the gold pieces I tested. I first tested the pieces for 14K and the deposit on the testing stone never did dissolve. I tested for 18K, same thing.
I then used the Platinum Test Acid on the pieces. The deposit did not dissolve, at all, or change color, that I noticed?
So I figured they were Platinum. I had already accidently put the pieces into a Nitric refine once before. They did not dissolve any that I noticed. I then put them back up in a seperate location for later.
Then this time they may have been put back into another Nitric refine, I had a good bit of alloyed silver that I put into this Nitric Bath this time thinking it was alloyed with gold. Came from an old Jewelry Store Auction, years ago. So there was a lot of Silver in with the pieces this time, not like the first time where just a very little silver was in solution. Then trying to research what to do, I found a post that said if you have a high silver content in the Nitric Solution, it (Nitric Solution) will try to dissolve Platinum. I ran this lot many times, for days. So, if they (Platinum Pieces) were in there, (Nitric Solution) they had plenty of time to dissolve this time around with all the silver in the solution as well.
I will do the test that you have previously recommended next week on stock pots to see if they test positive.
Question 1-Is Platinum noticeably mcuh harder than gold would be?
Question 2- Qst42know asked me if I had tested for Palladium, I haven't. Would these pieces have behaved the same way under the acid test that I ran if they were Palladium? Does Platinum and Palladium behave similar when being refined? I must admit I haven't had time yet to study the behavior of the Platinum group metals, yet. That's why I was saving these pieces until I finished up the gold I have. I have an old packhouse I used to put auction purchases in/and to get auction items together in. I keep running across Jewelry all the time I packed up years ago. So I have had more Gold Filled/Gold Jewelry to refine than I first thought I had. But anyway, I was going to study this group of metals in more detail when I got to the point of being able to refine them. I have all my used solutions, every last bit of them. I know I have made mistakes and I expected to make mistakes so I continue to save all my decants. So, I have the PM's somewhere, it's just that I got to find it.
I am going to sneak back over to the old house (while wife if gone) and give one more good search for the pieces. It would be good experience to go through the testing for the Platinum, but I am not quiet ready yet. I still have other refines ahead of this. So, I am going to make sure that I am not overlooking the pieces so my testing would not be in vain.
And yes Butcher, I have had to beg off and accept the responsibility of misplacing the pieces. She (wife) was only trying to help me. And as you said, she is always right, no matter what I think???
Thanks Butcher,
Oneal
 
Hi qst42know, thank you for your post.
Qst42know I haven't tested for Palladium yet? I am at the point of having done a HCL Boil on material. I must admit I haven't studied the Platinum group metals behaviors yet? Been too busy with gold refines.
Question 1- If these pieces were Palladium, would Palladium have dissolved the first trip through a Nitric refine? The pieces I had already survied a Nitric bath previously by mistake. Would Palladium have dissolved in the first Nitric solution if very little silver was present in solution. The difference in this time is that I had a lot of silver in this refine. I dissolved some sliver that was alloyed with gold in this refine? So there was a lot of silver present in the nitric solution this time verses very little silver in the trip through the Nitric Bath the first time?
Thanks Qst42know,
Oneal
 
Platinum must be alloyed with silver to dissolve in nitric. Silver in solution won't change that.

I have encountered a very old piece of gold over silver that tarnished so bad from co-migration you couldn't tell what it was. It looked like gold but survived an AR bath. If you hit one of these with AR (like platinum test acid) you would have produced silver chloride and may have drawn the wrong conclusion.

There are some side effects from poormans nitric that don't resolve easily.
 
I agree if these were silver, they may have dissolved in nitric, they also would not test for gold in chloride solution.
They may not have been platinum, but unless you find them we will not know for sure.

Like qst42know, says unless the platinum and 10 parts silver were melted together, nitric would not touch them (no matter how much other metal silver was dissolved with them in solution), unless they were silver or palladium (then nitric would attack them).

if you did not throw away any waste or material, if they valuable and were in the batch you can recover them no matter what valuable metal they were.
 
It should be noted that when palladium is a part of an alloy, unless it's present in miniscule amounts, it will discolor the solution badly. If it's present in a small amount, a solution that would have been blue would be green, and if it's present in volume, it may well turn out to be dark green through brown. So then, if palladium is present, it's usually very obvious. A quick test with stannous chloride is generally enough to reveal its presence, even in trace amounts. When all else fails, a test with DMG will usually be conclusive.

Harold
 
Thanks everyone for your post, I have been down sick again for the last few days. I never did shake that flu entirely and working late in the cold/rainy weather it's (flu) tried to jump back on me again. I can't go out and play, I am having to stay inside. This is (wife's order's) until I am completely well this time. I will have to admit though, that's all I feel like doing. When I am able to go out and play again I will let everyone know what the status of this is. But one thing I know for sure, I will take the flu shot ahead of next flu season.
But thank you all for your post, they are appreciated.
Oneal
 
Hi Butcher,
I have another problem that I just don't know what to do about. I follow your directions/instructions when doing a refine, I go through each and every step, sometimes an extra step or two depending on the condition ( how contaminated) that gold powders were in.
On this last refine while incinerating between HCL Boils, rinses before Nitric Treatment I over incinerated the powders and made some small balls of Gold. I have been trying to get the AR to dissolve these little balls of gold. After 3 treatments with AR I still have not dissolved them?
I feel that they (gold balls) have contaminates in them. I was going to run Harold's (Making Gold Pure) method as usual on the droped gold to clean out the impurities.
Would you inquart these little balls of gold and re-refine or hammer them really thin and treat with pure homemade Nitric or other? Or just put them in the dropped gold and re-refine the whole lot together?
One more thing, will I need to evaporate (strengthen) my homemade Nitric to treat these little balls of gold with if that's the best method to go with? I have been sick and am not thinking too clearly yet. Thank you for any advice.
Thanks Butcher,
Oneal
 
Oneal,
If these balls do not dissolve in aqua regia, will they dissolve in nitric? (I do not know the source of this gold, but could it have had some silver in these powders?

If your nitric is very dilute I would just heat it with metals the heat will help the metals to dissolve into solution and will concentrate the nitric at the same time.
 
Hi Butcher, thank you for your post.
This is another Gold Filled Jewelry lot that I am refining and this lot did have a good bit of silver in it. This is another one of the lots that came from a Jewelry Store sell out. There was a package that was marked (Alloyed with Silver). I did assume that this material was alloyed with gold but it could have been alloyed with something else? I have treated this Gold Filled Jewelry lot multiple times with Nitric, multiple HCl Boils also. I also went through the HCL Boils/Rinses with hot water, also added about 10 drops of sulphiric, then concentrated solution, dried, washed and incinerated again to make sure to drive off any acids. I got the powders too hot when incinerating the last time, resulting in making little balls of gold that will not dissolve in AR Treatments? I am just letting the AR solution sit until I can find out the best way to tackle this refine with the small balls of gold that I accidently ended up with due to gettig the powders too hot when incinerating the last time. The little balls of gold are in with powders that would not dissolve for some reason?
Butcher, I had a small amount of gold powders that I added to this lot. I had already dropped a previous lot of gold with Stump Out and washed several times.
I guess it is possible that I didn't get all the Sodium Metabisulfite completely out of this gold powder. If I did not get all the sodium Metabisulfite out of the powders that I added to this refine what would the indicators be if added gold powders contaminated with Sodium Metabisulfite to this refine before a HCL Boil?
Just wanted to know your thoughts on this refine before I move forward on the refine? Should I just drop the gold out of the AR now and then treat the little balls of gold in a seperate refine by inquarting or try and dissolve in pure Nitric. I will have to concentrate my Nitric and the salts that are left from Homemade KN03 is a concern for me and I wanted to ask you about it.
One more question, if you leave a container open to the air, will Nitric slowly work it'self out of a solution or do you have to drive the Nitric out of solution by evaporation or neutralize the Nitric? I guess what I am asking is, will HCL, H2S04, HN03, Etc;, slowly become neutral in a solution if you leave it open to the room temperature or will acids stay in a solution for extended periods of time until it is either driven off by heat or neutralized?
An important lesson I have learned on this refine is that you do not try and work when you are sick with the flu!!
Thanks Butcher for any guidance,
Oneal
 
Oneal58:

Howdy, I tried to dissolve two tiny pieces of platinum to make a standard solution. It took me over 8 hours to dissolve .1 gram of pure platinum!

Even then I did not get it completely dissolved - there was a tiny piece left over about 1/10 the thickness of a hair (approximately).

I added multiple doses of hot concentrated aqua regia.

Platinum if very difficult to dissolve!

Also, I harvested my first platinum metal today from two catalytic converters, please see:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=12455

Thanks - kadriver
 
I would treat these small balls, separate from the rest of the powders, if they would not go into solution (aqua regia).

I do not know what they are, much would depend on what metals these powders being incinerated contained, but if they would not dissolve in aqua regia, I suspect they could be high in silver or lead or some other metal insoluble as a chloride or that would passivate in the aqua regia solution. The platinum group can be very hard to dissolve in aqua regia (some of them will not dissolve in aqua regia), but from your descriptions I kind of doubt that is the problem, first of all considering the source, (unless this is your missing broaches), and secondly I would think that other metals would melt into balls long before this more noble metal like platinum would.

If these small balls were high karat gold they would dissolve into aqua regia.
If they were silver and gold melted together they may form a passive layer of silver chloride and not dissolve further. (And also may not dissolve in nitric because of gold), in this case inquartation would help.

There are very few metals or combinations of metals that would not dissolve into aqua regia.



I would wash these balls well and try nitric, if no luck there then, inquarter them with your next melt.

As far as acids evaporating in open air if stored in open air.
Much would depend on the concentration of the acid (water involved), the temperature, and what acid.

Many of these acids are made from gasses dissolved in water.

NO2 nitrogen dioxide gas dissolved in water forms nitric acid, (one of the more volatile acids), if it was concentrated it would fume off strongly we also call it fuming acid, even at 68% concentrations it will decompose slowly (again depending on temperature) gassing of NOx gases, nitric acid will also decompose in light. if the acid contains more water (more dilute), these gasses can dissolve back into solution easier as the acid decomposes, so less would be lost to fumes, storing in direct light would still try and decompose even a dilute solution.

HCl hydrochloric gas dissolved in water to form hydrochloric acid if the acid is concentrated say 32 % and the bottle is open it will release fumes of HCl gas, again temperature can have an effect on how fast the gas fumes off, a very dilute HCl these gases would mix back into water easier and not leave the jug so easily.


Sulfuric acid is usually SO2 sulfur dioxide dissolved in a water and H2SO4.
Sulfuric acid is not very volatile and would need a very high temperature before the SO2 gas would evolve, so mainly water would evaporate from the acid and it would concentrate further.
 
Hi Kadriver, thank you for our post. I have been down in bed with something I can't seem to shake. I haven't been doing any refining this week at all. Kadriver I haven't felt like following your post on your Platinum recovery but I hope to feel better in a couple of days and I will go through it. Did you find it was much more involved than the gold filled lots you have refined. Do you plan on pursuing the catalytic converter refining?
Thanks, Kadriver
Oneal
 
Hi Butcher, hope you are doing well. Been down this past week in bed entirely with a touch of pneumonia. I decided the best thing to do was to wait untill I am over this stuff before I go back into the cold and wet again.
Butcher, 1 thing I wanted to ask you, IF I accidently added some Sodium Metabisulfite between HCL washes what effect would this have had on the gold I was refinning? I added some gold powders that I had already dropped. I had washed the gold several times to get the Sodium Metabisulfite out. But after adding the gold I could smell the Sodium MetaBisulfite very strongly in the vessel that I used to add the gold to the larger lot. The reason I ask this is because it seemed like the looks of the refine I was working on changed. This happened between 2 HCL washes.
One other question Butcher, do some refiners use .925 sterling to inquart with? Or does that just add .075 other metals in with the gold you are inquating?
Thanks Butcher
Oneal
 

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