The atoms sue you for spying on them. ;DI would gladly do something like this - for few minutes, then lose patienceBut I will very much like to see that under good electron microscope.
THere, it would be probably the one and only place, where having impure and contamined precipitate would be more interesting and preferable - just to observe the few atoms of silver, gold and other PGMs just sitting there
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Bullion.Forum
Separating Pd and Ag from Tungsten filaments
- Thread starter bhaden57
- Start date
Help Support Gold Refining Forum:
Apologies I couldn't reply to this earlier because I changed my email and thankfully Frugal sorted this for me (Cheers Dave.)
4metals you're right this isn't the correct video. I'll try to find the one that's applicable.
anarxi
Well-known member
- Joined
- Oct 30, 2019
- Messages
- 420
perhaps it was the so-called “graphite”, silver sintered with graphite, a fairly common thing in automatic electrical switches and contactors...
Tungsten contacts are often found in low-current relays and vibration transducers. After nitric acid they remain quite shiny and can even be confused with platinum contacts.(pt/ir 10)
but after the fire they darken, sometimes a rainbow appears.
I also had sintered tungsten ones. I did XRF of them multiple times - insoluble residue after nitric. And I only seen tungsten + some very minor other elements.
I know about W-Al sintered pieces in diodes (these look like solid tungsten, but if you will do XRF, it will clearly see also Al). But this is different looking and behaving in acid.
But you answered main question and solved the issue - nitric won´t appreciably attack solid tungsten.
Abdoulapapatte
Well-known member
- Joined
- Apr 14, 2020
- Messages
- 103
hello a little word on this, also confronted with a treatment of large ingot of silver contaminated with W.
It was 60 kg of very badly foondu material, because W resists T° and has a much higher melting point than silver.
So you can take 65% nitric to start your treatment to start your wet etching (aqueous solution), it will simply look like a quartation or here the tungsten, would take the place of the gold, I simply mean that it will resist the nitric and you will see that if you handle your alloy by hand, you will feel a difference in density (like when you are at 50% of the work in Au/Ag quartation so your alloy is still there but you feel that it is less heavy and more friable.
If it's fairly homogeneous, of course. Otherwise the strongest parts will be those where you have a high concentration of tungsten.
And indeed you will see that the surface where the tungsten has resisted is as if scratched, less smooth than before, this is explained by the fact that the acid only eats away at the silver, and leaves the tungsten intact.
to then separate P de Ag several possible routes depending on your reagents, your possibilities and your knowledge.
to separate your palladium from your silver there are several solutions that come to mind.
1)
you have the Hcl + Ag solution -----> AgCl leaving your Pd in solution, but silver chloride is volatile and takes quite a long time to process. especially when it comes to filtration and cleaning. but you can get your silver out easily in 999.9/1000 if you are scrupulous about filtration and enemas.
(agcl wash x5 hot water) then treat it with NaOH and a saturated sugar solution.
2) you can recover Pd after nitric etching with Dmg, which is also very volatile and DMG is not given. it is generally used to recover traces of Pd and will detect it, and collect it even in very small quantities.
3) Here is the procedure I would use if I were you to go out
Age 999.9 and Pd 999/1000
a) inquartation , you must therefore add silver to be able to dip your filaments in the molten silver, the but is to cover them with the molten silver so that the silver takes the palladium with it (leaching by fusion) like the process of a coupellation for gold with lead.
b) Once all your filaments are well immersed in the molten metal, recover them with a stainless steel sieve big enough so that it doesn't melt when the molten metal passes through it. Basically, you're going to recover your filaments from the molten alloy.
or when you go shot blasting you can simply put the stainless steel filter (or titanium even better) the molten metal flows into the water and the filaments are retained by the filter.
Don't use lead here, but silver if you have it, because lead chloride will be annoying for the rest of the process, or you'll have to do other steps not covered here.
c) You will then make an Ag/Pd alloy and the filaments will be freed from what interests us here (Ag and Pd).
-------------------> output of pure W
d) take your shot if you have shot blasted it's better because larger surface exposed to acid so faster digestion. Or if you have a ball of alloy (as after coupellation), or an ingot (because you have ingotted) from which you have just removed your filaments, you will have to laminate them (make thin plates by crushing the metal with a laminator).
-------> All these steps are not necessary if you manage to attack Pd and Ag with nitric directly and your filament comes out clean. so take a sample and see if it's possible, but combine them with silver, during melting, the silver can help you take everything if you can't, and at that point you will have recovered 100% of what interests you, know that wood is known to be an enmmerder No. 1 that tends to annoy professionals because very difficult to treat with precious. <------------------
e) you can now attack the nitric HNO3 by heating your solution.
d) Once it has been digested, filter it.
f) It's time to take out the silver, use HCl and separate the white AgCl from your stock solution.
------> formation of agcl -----> oxidation with NAOH-----> reduction with 1 saturated sugar solution.
-------------------> output of pure Ag
g) Add NH4 (ammonia) 12% or 20% you must go quickly in this step, or else a called VOKELEN'S SALT may appear nothing serious and if it appears you just have to filter it. put it aside for further treatment by calcination, or re digestion by acid (going from a brown to a pink violet colour).
h) It is now time for you to precipitate your palladium by adding HCl to your solution which you will have cooled beforehand (the colder your solution is beforehand, the quicker the formation of a yellow precipitate will appear), at this stage you must go slowly, adding little by little, do not add more HCl than you need, I advise you to take a small part of your solution to be treated and to carry out tests to know exactly how much you should put in. To make things easier for you at this stage too, you can start with 37% HCl (muriatic acid) and when you think you've precipitated everything continue a little with dilute HCl.
i) The precipitate you will see is called palladium diamine dichloride (100% pure).
j) recover the yellow precipitate by filtration and wash it with dilute hcl. Recover the filtered liquid and test it with stannous chloride, if the presence of Pd is detected, add a little DMG to recover traces of Pd.
k) Recover your yellow precipitate from your filter, which you have washed well with dilute HCl, and place it in a beaker, add water and start heating your mixture. Once it has disintegrated in the water, add formic acid little by little, and you will see that a foam appears on the surface of your mixture, which is a good sign.
l) your palladium will precipitate in pure metallic form, I guarantee 999.9/1000 if you have done your procedure correctly. if you need a video tell me and I will search the internet for you.
comments: all the procedures I give are checked and I carry them out before talking rubbish on a forum, it's not just about a little, it's validated with lab tests and analysis of my results, no nonsense in what I tell you ok, you can go, I passed the ton of gold a very long time ago. I don't know everything and I'm sometimes a real chip off the old hoot in certain areas, I came from a STL science and technology laboratory course, specialising in biochemistry and biological engineering. I don't know if it's the onset of Alzheimer's or the fact that I stopped studying for 12 years, but at the moment I can't remember anything, I can't give you the atomic valency or find the spdf sub-layer of an atom. But I've got some nice leftovers, trust me for my procedures. I'll find a video that talks about it by searching a bit on the net if you want and like me you prefer to see a process rather than imagine it.
I hope I've helped you my friend, bye.
It was 60 kg of very badly foondu material, because W resists T° and has a much higher melting point than silver.
So you can take 65% nitric to start your treatment to start your wet etching (aqueous solution), it will simply look like a quartation or here the tungsten, would take the place of the gold, I simply mean that it will resist the nitric and you will see that if you handle your alloy by hand, you will feel a difference in density (like when you are at 50% of the work in Au/Ag quartation so your alloy is still there but you feel that it is less heavy and more friable.
If it's fairly homogeneous, of course. Otherwise the strongest parts will be those where you have a high concentration of tungsten.
And indeed you will see that the surface where the tungsten has resisted is as if scratched, less smooth than before, this is explained by the fact that the acid only eats away at the silver, and leaves the tungsten intact.
to then separate P de Ag several possible routes depending on your reagents, your possibilities and your knowledge.
to separate your palladium from your silver there are several solutions that come to mind.
1)
you have the Hcl + Ag solution -----> AgCl leaving your Pd in solution, but silver chloride is volatile and takes quite a long time to process. especially when it comes to filtration and cleaning. but you can get your silver out easily in 999.9/1000 if you are scrupulous about filtration and enemas.
(agcl wash x5 hot water) then treat it with NaOH and a saturated sugar solution.
2) you can recover Pd after nitric etching with Dmg, which is also very volatile and DMG is not given. it is generally used to recover traces of Pd and will detect it, and collect it even in very small quantities.
3) Here is the procedure I would use if I were you to go out
Age 999.9 and Pd 999/1000
a) inquartation , you must therefore add silver to be able to dip your filaments in the molten silver, the but is to cover them with the molten silver so that the silver takes the palladium with it (leaching by fusion) like the process of a coupellation for gold with lead.
b) Once all your filaments are well immersed in the molten metal, recover them with a stainless steel sieve big enough so that it doesn't melt when the molten metal passes through it. Basically, you're going to recover your filaments from the molten alloy.
or when you go shot blasting you can simply put the stainless steel filter (or titanium even better) the molten metal flows into the water and the filaments are retained by the filter.
Don't use lead here, but silver if you have it, because lead chloride will be annoying for the rest of the process, or you'll have to do other steps not covered here.
c) You will then make an Ag/Pd alloy and the filaments will be freed from what interests us here (Ag and Pd).
-------------------> output of pure W
d) take your shot if you have shot blasted it's better because larger surface exposed to acid so faster digestion. Or if you have a ball of alloy (as after coupellation), or an ingot (because you have ingotted) from which you have just removed your filaments, you will have to laminate them (make thin plates by crushing the metal with a laminator).
-------> All these steps are not necessary if you manage to attack Pd and Ag with nitric directly and your filament comes out clean. so take a sample and see if it's possible, but combine them with silver, during melting, the silver can help you take everything if you can't, and at that point you will have recovered 100% of what interests you, know that wood is known to be an enmmerder No. 1 that tends to annoy professionals because very difficult to treat with precious. <------------------
e) you can now attack the nitric HNO3 by heating your solution.
d) Once it has been digested, filter it.
f) It's time to take out the silver, use HCl and separate the white AgCl from your stock solution.
------> formation of agcl -----> oxidation with NAOH-----> reduction with 1 saturated sugar solution.
-------------------> output of pure Ag
g) Add NH4 (ammonia) 12% or 20% you must go quickly in this step, or else a called VOKELEN'S SALT may appear nothing serious and if it appears you just have to filter it. put it aside for further treatment by calcination, or re digestion by acid (going from a brown to a pink violet colour).
h) It is now time for you to precipitate your palladium by adding HCl to your solution which you will have cooled beforehand (the colder your solution is beforehand, the quicker the formation of a yellow precipitate will appear), at this stage you must go slowly, adding little by little, do not add more HCl than you need, I advise you to take a small part of your solution to be treated and to carry out tests to know exactly how much you should put in. To make things easier for you at this stage too, you can start with 37% HCl (muriatic acid) and when you think you've precipitated everything continue a little with dilute HCl.
i) The precipitate you will see is called palladium diamine dichloride (100% pure).
j) recover the yellow precipitate by filtration and wash it with dilute hcl. Recover the filtered liquid and test it with stannous chloride, if the presence of Pd is detected, add a little DMG to recover traces of Pd.
k) Recover your yellow precipitate from your filter, which you have washed well with dilute HCl, and place it in a beaker, add water and start heating your mixture. Once it has disintegrated in the water, add formic acid little by little, and you will see that a foam appears on the surface of your mixture, which is a good sign.
l) your palladium will precipitate in pure metallic form, I guarantee 999.9/1000 if you have done your procedure correctly. if you need a video tell me and I will search the internet for you.
comments: all the procedures I give are checked and I carry them out before talking rubbish on a forum, it's not just about a little, it's validated with lab tests and analysis of my results, no nonsense in what I tell you ok, you can go, I passed the ton of gold a very long time ago. I don't know everything and I'm sometimes a real chip off the old hoot in certain areas, I came from a STL science and technology laboratory course, specialising in biochemistry and biological engineering. I don't know if it's the onset of Alzheimer's or the fact that I stopped studying for 12 years, but at the moment I can't remember anything, I can't give you the atomic valency or find the spdf sub-layer of an atom. But I've got some nice leftovers, trust me for my procedures. I'll find a video that talks about it by searching a bit on the net if you want and like me you prefer to see a process rather than imagine it.
I hope I've helped you my friend, bye.
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