refining white gold

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That is nice to know, that you can lose gold values in the silver. I was always focussing on getting the silver out of the gold, if there was any. Thanks. And solar, you are right, I should show a little more gratitude to those trying to teach me new things. I am sorry, and really have learned something from each and every reply.
 
Ok, first time with white gold, and I have discovered much. I made enough mistakes that now I have to redissolve the whole batch. It seems there was rhodium, and in my attempts to heat it enough to dissolve, some of it did. Now my gold precipitate is mixed in with a bloody colored solution, which settles after a while. At first when I saw the brick red precipitate I thought it might be palladium, or is it platinum. But it soon turned the color of dark red blood.
Should I just redo the whole batch in cold AR and then figure out what to do with the red stuff? I don't know if it is an insoluable rhodium salt. How do I turn rhodium salt back into it's elemental state?
At least I know everything is still there. Even though it is getting squirelly on me, I still want to learn how to do white gold by itself. I am finding it is better to separate my gold a little better, and not try to refine the same way I do my laundry.

Next time when the gold is done, I leave whatever didn't dissolve alone, collect it, and do a batch of that some other time.
 
If your dealing with white gold then chances are their is some Pd present. Now i would like to point out again the benefit of inquarting. Had you inquarted the Pd and Pt would have been removed before the Ar process. When alloyed with silver Pd and Pt will dissolve and follow the silver into nitric. After the nitric step you would have been refining nearly pure gold making you job a lot easier and the recover and segregation of the metals a snap. The whole process should be completed in an 8 hour process from start to finish at the most.
 
WOW!!! I never looked at quartation in that respect. Thank you for a HUGE lesson! And humility is part of it too butcher.
 
Actually, that "thankyou" was meant for you Solar as well, especially after the part about Pt and Pd following the silver into the nitric. I will refresh my Holkes to see if she says how to get the PGMs out of the nitric. Silver is easy. On that note, has anyone ever tried adding silver chloride, tin and sulfuric acid together? I am curious if the tin would take on the Cl from the silver, or would that just give me silver sulfate and tin chloride?
 
Palladium said this Pd-Pt-thing. That was also new to me. :lol: But okay, in my very special way, I am great, too. 8) I am great in asking annoying questions,for example. :lol:
 
Solar you are truly great in your special way.

au-artifax,
I think you too have grown, and earned my respect for you as a fellow member, with your humility you have actually raised yourself to a higher level in understanding and respect from others, with this minor step you have put yourself on to the course of becoming a better refiner and forum member, and an all around greater person.

Funny the very thing our pride seeks, the ego pride destroys, the very thing our Ego fears, is that that we can truly be proud of.

We as humans are very funny creatures with our prideful egos, the very thing our ego fears,and can help us grow, is actually what can make us proud of ourselves, Humility, is actually the thing we need to grow and to gain us respect, to be able to be truly proud of ourselves.

It is very hard to learn, until we can admit to ourselves we do not know.
 
when nobody esle would take the time (actually
most of the guys were looking at there appointment
book trying to find an empty few hours for you)
i come running to your rescue ,probably took
3 hours out of my game playing and then had to
recharge my phone so 4 hours

but do i get more respect ,do i get to have an ego
no i just get pushed aside

the info that paladium gave you is second hand
news i could have told you at the getgo but didnt
think you were ready for it..... What ....what's
everybody looking at ..........really

all jokes aside i am glad you have found your
way

steyr223 rob
 
Well thanks. I want to get some ideas here, on how now to deal with these mixed precipitated. I can think of some for sure methods: A.....redissolve all in AR then precipitate pt, pd then au in that order (I actually went through the processes to drop pt andpd but think my solution was not boiled down enough... Or I didn't wait Lon enough... Or I didn't add enough ammonium chloride or chlorate....whatever.)
B.....go ALLLLL the way back to the inquarting process;

C.... I had an idea that if I try redissolving JUST the au with AP, I could get a good separation (I figure this might save materials).

Does anyone have any opinion on this they can share? I have plenty of time, haven't really lost metal values....just trying not to lose much more time .....not to mention.... Losing something that will cascade into losing the most.... My patience!!!
 
you may have a better outcome to precipitate gold first. ferrous sulfate mixed with the solution will bring down mostly gold. this leaves the last two. after you condense the solution by evaporation, ammonium chloride is added to precipitate the PGM's. palladium can be removed from the incinerated powder with hcl boil.
 
The more efforts one already has invested into a mistake, the more unlikely one will be able to stop. I learned this, when I studied some years MA in social behavioral sciences ( well, I did stop,before I got MA, but those studies were only a hobby to me like refining now, - beside my work). But I think, to be aware of this effect, could help you in your decision. I would try not to let me lead by the emotions now, but carving objectivity. Take the most proper way, although it will cost some patience.

I am curious what our masters of refining will say, is the most proper way. I just saw that Geo already has answered and he is one of those,who know, what they are talking about. Just a question....would going back and do the inquartation not be the most proper way?
 
yes, i do apologize for not adding that its just my opinion. im sure there are a couple different better ways but my meager understanding of the subject (ive only actually done it a couple of times myself). i was assuming it was already in solution.
 
The timeline for this fiasco went like this: dissolved jewelry in AR and decided to throw in some white gold. Saw silvery flakes not dissolving so I cranked up the heat on the AR. The flakes never fully dissolved so I filtered them out. There was no silver chloride in sight and the solution was a green tinted but on the yellow side. To remove the nitric I did a combination of saturating the solution with gold and evaporating it down. I added some ammonium chloride to see if anything would precipitate and nothing,(not realizing I did not condense the solution after reconstituting it with dilute hcl). Then potassium chlorATE and nothing came down. Then SMB.... and lots of precipitate....more than I expected.
Wash wash wash in h2o, wash wash wash in hcl, wash with ammonium hydroxide, wash wash wash with water, then hcl, then wash with water.
In the middle of all this washing the solution turned blood red and the precipitate like powdered brick. That's where it sits...a mixed precipitate of gold, platinum, palladium and rhodium. Hey, at least all the values are still there, without the base metals. (I am sure the ammonia stripped away any chlorates of silver and copper long ago
So that's it in a nutshell.
Notice that I never inquarted.....(yes...he can be taught)

Hope that clears up any vague points. Seems I dragged all the PMs down at once.
(Sticky wicket)
 
So going Alllll the way back would be melting it all down with (I estimate 6 oz of silver, but seeing as it's no longer karat gold, do I use the full 3/1 ratio of silver/gold?), then nitre-out the silver/platinum/palladium. The gold drop is easy enough, But what do I do with the Rhodium? I dont have a fussion furnace to process rhodium the right way.
Do I go after the PGMs the same as if it were done in AR after dissolving in plain nitric, (after having added hcl to the filtered solution to bring down silver chloride...then filtering again). Would the adding of hcl create AR at that point and the solution now take on the pt and pd?
 
If these powders were mine I would consider, Incineration of the washed and dried powders,to remove traces of previous acids and compounds, then treat them first with dilute HNO3 to remove any base metals, silver and palladium, then go after the gold, if working without heating the solution strongly not much of the platinum would go into solution, since this is already powders not much reason to in-quarter at this point, unless for some reason you wished to collect platinum with the silver, and unless this was a very big batch I do not think their will be enough PGM to mess with, saving the insolubles till you get enough PGM to mess with or sell, and collecting the traces from solutions in your stock pot.
 
We are sorta on the same wave pattern. Today when I had siphoned off all the liquid after another wash I had my hotplate on and started getting ready to roast the precipitated. I stopped though, questioning whether it mattered that I didn't do the last wash with distilled water. That's what I was getting ready to do.

But now that I heard how it sounded coming from you, I think that is what I am going to do....(what you would do). The only dded thought I had was that following the predure you laid out, with the mix I have, is that I don't have to worry about the Pt because it, along ith the rhodium will be the only thing left in the vessel right before I strain it and grab the gold out of the filtered solu
tion.

There definitely is not enough yet, like you said, to go after those two...(three if there was any chance of iridium, but very doubtful) the Pt and Rh. Question though....about the Pd.... If it's mixed with the silver in the hno3, and I put hcl in to precip silver, then the filtered solution I treat like regular AR?
funny... My mind is spinning because I am thinking way ahead of myself here. I need to collect a lot more PGMs before it would be economical to use materials up like that. And a huge inefficiency on my part.
Well thanks again though. Tomorrow I will roast my powder.
 
Before roasting silver or gold that has seen chlorides, I will normally wash them in dilute NaOH solution this forms NaCl salts of any chlorides, which can easily be washed with water, this is a precaution as silver and some gold can become volatile if roasted with any chloride salts.

The nitric will dissolve base metals silver and most of the palladium, silver can be precipitated as a chloride with either table salt NaCl or HCl this will leave palladium in solution, problem is the silver will need converting back to metal before melting (silver chloride is volatile and will burn up most of it as white smoke) silver can be converted with the NaOH Karo syrup method or with one of the acid and metal methods to replace silver from solution.

This will leave most of the palladium in solution. which can be recovered by several methods, cement out out palladium with copper (probably easiest), or zinc (cements out several metals), you can also evaporate the solution down several times adding HCl with each concentration to change the palladium to a chloride, then NH4Cl, and small additions of sodium chlorate to precipitate pd from boiling hot solution (trouble some procedure), or using DMG, dimethyl glyoxime is not only costly reagent, and forms very voluminous solution, for this reason DMG is normally better to test for palladium than a recovery method. and with small volumes you can always just collect palladium in one of your stock pots.

As with the other PGM's what metal you chase after now or try to recover later from the stock pot or silver pot, can be determined of how much of these metals are actually in solution, many time it is easier to keep healthy stock pots and accumulate these metals until you have enough to make a recovery of them, chasing traces will also loose some of the small traces, and you may not have enough to amount to anything recovered, while saving them up in the stock pot letting them accumulate to larger volumes, it may be easier to recover and also you may not loose as much in
the long run.


The Platinum groups are similar in nature to the in that they are hard to separate completely,
they for them most part are more difficult or if not almost impossible to put into solution.

Palladium will not dissolve easily in aqua regia, but it will dissolve into HNO3 alone, or HCl alone fairly easily, (Hoke's speaks of dissolving the palladium in HCl first before adding HNO3 to form the aqua regia to put the other metals into solution with the Pd, otherwise it would be hard to get the palladium to dissolve into the solution with the other metals).

Platinum will dissolve in very hot aqua regia,but can take a long time to dissolve, if powders more easily than the solid metals, but still difficult, gold will dissolve into a cold or barely warmed solution of aqua regia (if not alloyed with silver, or in a high alloy of PGM), gold powders also dissolve much more quickly than solid metals, this gives us a way to dissolve gold away from platinum with out putting much platinum into the solution.

Iridium also dissolves very slowly if at all (incineration can actually help to make it more insoluble depending on previous treatments), you could then cover the powders with adding HCl first, then adding HNO3 ,and heat the aqua regia strongly, to put base metals, palladium, gold, platinum, iridium would dissolve very slowly if at all, Rh is almost impossible to dissolve into this solution.

But then again with most of these PGM's unless you have processes an awful lot of dental gold or jewelry with these metals involved you most likely will not have enough to mess with, so the stock pot method as taught in Hokes book is one way to keep a good little piggy bank.

Keep studying Hokes book, there are different ways you could go about recovery of these metals, and many times the choice you may choose can be decided when you know the conditions you are faced with, or materials and their conditions, as with different situations you face different challenges of recovery, separation, or refining.
 

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