Palladium

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jimdoc,

In the late '70's, I ran a bunch of Balfour class rings called, QPal. The Q stood for quarter or, 25% palladium. They were made for people that couldn't afford gold. They were very hard. I would guess that the other metals were copper and nickel, similar to the clad coinage. The ones you have are very likely the same alloy.
 
I found this on eBay. According to this guy, Palladium Plus is 25% palladium and 75% sterling silver. I was half right. It seems that the silver was the "Plus."

http://cgi.ebay.com/Ryder-Truck-Safe-Driver-Ring_W0QQitemZ110099149356QQihZ001QQcategoryZ10963QQcmdZViewItem
 
25% palladium 75% silver is known as precium. That guy in the Ebay ad states they are palladium plus quality, he doesn't say they are stamped
Palladium/Plus. That ring is more like Precium quality or alloy.
I forget what company made the Palladium/Plus rings, but I looked through the catalog when I was in school and never ordered a ring because that is when gold was at record highs. I had never heard of palladium, or what they said was alloyed with to make it Palladium/Plus. I will use some nitric and find out for myself and let everybody here know what my results are in the near future. Thanks
 
Steve,
I got outbid on that one.
I think they are at least 90-95% palladium
and either ruthenium or silver alloyed or rhodium
plated. I just can't find any info on Palladium/Plus.
Here is a link from Stillwater on palladium;
http://www.stillwaterpalladium.com/jewelry.html
 
It seems this must be some sort of tradmarked name. Perhaps the us patent office or trade mark office could help? Do you have any info on the manufacturer (hallmark symbol) ?
Steve
 
No hallmark, just the Palladium/Plus stamping that you can see
in that auction. I also have one marked P+ that I think is the same
material. I think that one has a co. name.
The catalog we looked through in high school was from a big co.
like Jostens but I am not sure. I have searched everywhere for
info on P/P but can't find it. I guess there is only one way to
determine the composition for sure, use some nitric.
 
here's a link for an interview with some palladium manufacturers


http://www.dellsfinejewelry.com/palladium.

There is also some good info with the Bureau of Standards. I lost the page when my network blinked.

Steve K
 
Has anybody ever processed the multi layer ceramic capacitors for the palladium? and if so is there a way to determine the better ones?
I have seen Steve's writings and pictures on the monolith's and have a bunch of them to process, but I have a bucket full of the larger ceramic
ones, and I am curious about those as to why they haven't been mentioned here. I plan on experimenting with them soon, but recomendations and tips are always a help in going in the right direction.
Thanks. Jim
 
To get the palladium out of the monolithic capacitors, I have an idea. I presently have no way of trying it and wonder if someone else could. Here's the ones I mean. We always called them chip capacitors.
http://goldrefiningforum.com/phpBB3/viewtopic.php?t=51&start=30

As I understand it, the way they are made is to coat very thin layers of ceramic with a palladium thick film paste. The layers are dried, sandwiched, and fired. If the paste is the same as other PM thick film pastes, it contains a 5% glass frit. I believe the ceramic also contains a glass frit. When fired, the glass melts and bonds everything together.

The terminology I use for many parts is much different than the official names. There is a very common part I call ceramic cerdips (I know that's redundant). They are nearly black and are seen in various sizes. They are made with 2 rows of leads and with 2 ceramic layers bonded together with glass. We used to break them apart by heating them to about 800 deg F and then quenching them in water. This shattered the glass and they just fell apart. We then tumbled them together, by themselves, in a cement mixer and separated the kovar with a magnet. We then dissolved the gold from the pad on the ceramic with aqua regia.

The capacitors are also held together with glass, I think, and I wonder that, if they were heated and quenched, would they fall apart? Or, at least, be weakened enough so they could be more easily crushed or mashed or ground or tumbled to separate and expose all the layers. It might be best to remove the solder first before heating. The molten solder could cause a mess. If this is silver, as it was on most of these that I've played with, nitric acid would work. However, if they're silver, the melting point may be above 800 deg F. and they wouldn't need stripping. Maybe not, though. If lead/tin, I think a hot, dilute (about 7/1) muriatic would work.

To get to the palladium, the layers must all be exposed. This can be done, as is, by fine grinding. However, to expose all of the Pd layers, in this manner, isn't that easy.

Once all the layers are exposed, in whatever manner, the Pd could simply be dissolved in nitric. If nitric was first used to dissolve the silver solder, it should also contain a little Pd.

It would be a simple matter to try this out. Maybe, 800 F isn't the best temp. Also, the ceramic is an good insulator and will have to be heated for a period of time to get hot all the way through. Please let me know what happens.
 
I have finally started to mess with the palladium contacts from the Hammond organs I have been dissecting. I put the tips in 65% nitric
and it ate up the copper but not the palladium wire. This happened in
my smaller scale test also, but I was using 14K testing acid that is kind
of old, so I figured it may have been because of that.
My question is; Shouldn't the palladium wire have been dissolved also?
I still have it sitting now, waiting to see. I didn't use any heat because the acid really heated it up on its own. Getting rid of the copper is good, and was my first concern, but in wanting to refine the palladium also I was looking for that to go into solution also. Would using urea to neutralize the nitric work, before testing the solution for any palladium in it.
I was wondering if maybe the palladium wire was alloyed with any platinum that would make it not dissolve in nitric? Hammond ads that I have seen state the wires are "pure palladium" that is what got my interest in scrapping them for the metal, but maybe they alloy it for extra durability?
I finally got my tenth organ and was hoping to have over 20 dwt from the buss bar wires, but ended up with 19.1 dwt plus whatever I get from the trimmed off contacts since the last organ I got was another S-6 with only one small row of keys. Thanks. Jim
 
jimdoc said:
Shouldn't the palladium wire have been dissolved also?
Click to expand...

Yes, but not as quickly as copper or copper alloys. If you have a low acid content, the dissolved palladium will precipitate on the remaining copper (or copper alloy) as a black powder, so it's possible you did dissolve some, and it was left behind. If your solution went from green to blue, that's a good sign it happened. Be certain to check your solutions before discarding if they're not sky blue. Even then, check for traces of silver and other values, but don't expect much.

Getting rid of the copper is good, and was my first concern, but in wanting to refine the palladium
Click to expand...

Right. In order to precipitate clean palladium, you need to eliminate as much of the base metal as is possible. The alternative it to calcine the salt, then reprocess. It can also be dissolved with ammonium hydroxide and re-precipitated with HCL---but I wasn't too thrilled with that process, so I did it only once. The salt, which is a deep red in color, precipitates as a yellow powder by this process. Given enough time, I'll post a picture of some palladium, salts, and calcined salts eventually. Just have to get around to it. Haven't taken the picture yet.

So then, take advantage of what I said, above. Dissolve maybe half the copper, then stop. Allow the solution to sit long enough for the dissolved palladium to precipitate on the remaining copper. As it does so, it will dissolve some of the copper. When the solution tests barren, discard the solution and start with a fresh batch of acid. Not too much, just enough to dissolve more of the copper, without dissolving all of it. Repeat the previous operation. Do this until the remaining copper is very scant-----then dissolve the palladium, filter, and recover with ammonium chloride and sodium chlorate. It's done hot, not cold. Be careful to not lose the black powder when you decant the solution each time. Use a short length of vinyl hose, pre-filled with water and capped with your fingers. It works great, and you can control the flow by the difference in height of the discharge and intake of the hose.

I was wondering if maybe the palladium wire was alloyed with any platinum that would make it not dissolve in nitric? Hammond ads that I have seen state the wires are "pure palladium" that is what got my interest in scrapping them for the metal, but maybe they alloy it for extra durability?
Click to expand...

I doubt that they wouldn't mention the platinum if it was included. Palladium doesn't dissolve as easily as copper, but the addition of a little HCL changes all that. It readily dissolves in AR.

Harold
 
Harold,
Thanks for your answer. I am running out the door to go down the shore
and catch a concert, so I will check everything out when I get back. I saved all the solution, and the palladium wire from the tips all seemed
intact minus the copper it was attached to, but I think some must have gone into solution. I got 6 grams from about 2 ounces of tips, half of the tips had alot of copper because they were the newer type contacts that
weren't as skinny where the contact wire was. I plan on using this 6 grams
to experiment with getting into solution, and when I get it right I will do the rest of my wire and make an ingot or bar. Do you have any tips for that? I have read about palladium absorbing oxygen,sounds like I should stick with gold to learn casting first?
Thanks. Jim
 
If they were pure palladium, you could have dissolved the copper away from them with HCl. Hot HCl will also dissolve any nickel backing on the points. Check the points with a magnet to make sure all the nickel is gone. This way, you would end with pure Pd without dissolving any of it.
 
GSP,
I think the nitric worked jsut like you said the HCI should, I ended up with the contacts, which are just small snips of palladium wire tack welded to the copper. I thought it would all go into solution, but it didn't and if I knew that I would have saved the nitric. There should be no nickel, because of the 'wire' contacts. There are other bigger contacts that look like typical contacts from in the organ also I have to check, if they are palladium they should add up, but they may have nickel in them.
Jim
 
I've run a lot of old telephone wire relays that have pure palladium points. They look like they're made with very short lengths of thin wire, with flattened surfaces. Every pure Pd point I've seen looks like this. It sounds like your points are similar. We selectively dissolved the copper with hot concentrated sulfuric acid plus chromic acid and thought that only pure palladium remained. We tried nitric first, both hot and cold, but it always dissolved a little palladium.

The first time we sold them, about 100 ounces, the buyer dumped them out on the table to look at them. He saw a small metal staple in the pile and grabbed a magnet to remove it. When he removed the magnet, it picked up a huge clump of points. An unpleasant surprise. We looked through a microscope and discovered that there was a thin magnetic nickel backing on the points, although you couldn't see it with the naked eye. We removed the nickel with hot concentrated HCl. Check them with a magnet.

From my experience, I would bet that you dissolved some Pd in the nitric, especially if you totally dissolved all the copper. Due to their relative positions in the electromotive series, copper will tend to dissolve before palladium. However, when the copper is almost gone, the palladium will start dissolving. After all, the standard solvent for palladium is nitric acid.

Use stannous chloride to test for palladium in a drop or two of the solution. If palladium is present, it will produce a brown-yellow color.

Anytime you have pure solid palladium (or any other pure solid platinum group metal), you should avoid dissolving it, since it will be very, very difficult to get it pure again. Try to select a solvent(s) that will dissolve everything but the palladium.

One time, we ran a 50,000 pound (including the plastic relay cases) batch of these telephone wire relays. They ended up being worth about a dollar per pound, since palladium was worth only about $60 per ounce at the time. Today, they would be worth about $6 per pound.
 
jimdoc said:
GSP,
I think the nitric worked jsut like you said the HCI should
Click to expand...

The difference is HCL won't dissolve palladium. It will, however, dissolve palladium oxide, so regardless of the choice made when removing base metals, you should check your solution for values.

Harold
 
jimdoc said:
I plan on using this 6 grams to experiment with getting into solution, and when I get it right I will do the rest of my wire and make an ingot or bar. Do you have any tips for that? I have read about palladium absorbing oxygen,sounds like I should stick with gold to learn casting first?
Thanks. Jim
Click to expand...

I've commented on this before, but to this point it hasn't been an issue.

Understand that the platinum group is very unlike gold in that it will NOT precipitate well, if at all, from dilute solutions. Even then, it often will not precipitate completely, so your processed solution will still test positive. You may have to recover the traces on scrap metal and include the black powder in a future batch.

To precipitate, you'll want your solutions as concentrated as is convenient. If you've not done any of this before, I strongly recommend you read Hoke on the recovery of palladium.

I didn't melt much of my palladium, although I melted enough to know how it reacts. I simply calcined the salts to sponge, and stored the sponge.

Palladium, unlike platinum, reacts with oxygen readily. You'll see that when you calcine your palladium salts. They end up covered with the most beautiful peacock colors of green, blue and red. Hoke suggested that a fast wash with alcohol prior to melting would reduce the oxides, which I tried. It wasn't real obvious that it was effective, but I achieved respectable results in melting to a button.

I simply torch melted what few times I did anything with the palladium sponge. I allowed the button to form in a melting dish and removed it after cooling enough to set, but before the partially melted dish glued the button down. The button was then pickled with acid to clean it well. to be perfectly frank, I do not recall what acid I used, but for platinum, HFL was used, in a platinum container. It should be avoided like the plague by those that are not well versed with handling acids----it's a killer.

Aside from one tiny button that I will, hopefully, include in a future picture of the various states of palladium, I no longer have any of the buttons, and only a small vial of the sponge. It was all sold some time ago when palladium went up in value.

I recommend you do not try to learn about casting ingots with palladium. For one, you're not likely to encounter enough of it to gain much experience, and it melts at, roughly, 850° higher temperature than gold does (I'm trusting memory here, so I could be off a little). It's not pleasant to melt, unlike gold. You might consider simply creating buttons, as I did. It's the course of least resistance, and adequate. I'd suggest you investigate the high temperature melting dishes provided for the jewelry industry for melting the Pt group. Those nice little clay dishes I recommend for gold aren't an acceptable choice because of the high temperature involved.

Harold
 
Thanks GSP and Harold, I appreciate the info. The solution was bluish green so it should have palladium in there. I will find out when I get home.
I will be happy with a bottle of sponge also, untill I get enough material and experience with what I am doing.
Jim
 

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