# good problems



## Naitsabes (Aug 15, 2007)

I have a problem.

But it is a good problem.

I have two lots of scrap.

The first is a powder and foils - these were obtained from one of my treasure hunts here at Oak Ridge home of the atom bomb.

If you remember bizarro world from the superman comics well bizarro world would go a long way toward describing Oak Ridge TN.

So don't dismiss that which I say offhand.

I could tell other stories but this is this story.

A couple years ago I took these foils to a friend who runs a scrap yard and he had a hand held xray fluoroscope - this device suggested I had a mix of palladium, silver and rhodium in this material.

The rhodium indicated was rich enough so that I could have retired.

So I sent this off to a refiner for analysis.

Less than one percent rhodium and no palladium - not worth refining - they sent back my material in the form of a black grey powder.

Last week I was privileged to take the radiation Safety Officer Course at Oak Ridge Associated universities.

This institute is staffed by some of the worlds best experts in the use and abuse of radiation.

I mean the best the folks who figureed out how to do this stuff in the first place.

In the basement they have a setup for xray fluorescence.

They were absolutely delighted to analyze the powder I had received back from the refiner.

This setup was not intended to return percentages so I have no quantitative data only qualitative.

Four elements were returned (this setups crystal was not able to detect the return from rhodium by the by)

Tantalum, Zirconium, Platinum, and gold with platinum and gold giving the highest peaks suggesting the greatest concentrations.

I suspect the Zirconium and tantalum are in their oxide species due to teh black color of the powder but I have no way of knowing for sure.

So?

What to do?

Should I go back to a refiner and say how about gold and platinum?

Or should I try to do a bit of refining on my own?

And who would take the results of my efforts?

The other problem has to do with bases of a number of deware flasks I purchased off an Oak Ridge National Lab auction.

These are the dewares that look like they would be the greatest beer glasses ever talk about keeping your beer cold.

(I think the glass is plated with rhodium in these flasks.)

I noticed there were two types of bases to these flasks.

The first was obviously aluminum and quite corroded.

The second was apparently from the same lab but of a shinny white metal that was not corroded - takes a high polish does not react to nitric, hydrochloric, or AR.

Further on my salvage buddies xray shows gold, rhodium, silver, and iron as constituents - I had them shoot this again today after their machine had just been out for calibration.

I have hundreds of grams of both materials.

What to do?

I am almost a total neophyte at refining.

Is there a refiner I can trust?

At least the guys who powdered my first set of foils seem to have sent back the real stuff - their lab was apparently just fixated on rhodium and palladium.

Anyway they said the lab would only analyze for what was ordered and of course if there was any rhodium at all one might expect platinum.

Nice problem, huh?

And help!


----------



## lazersteve (Aug 15, 2007)

Got any photos?


----------



## Naitsabes (Aug 16, 2007)

Well its not much to look at but I took these images this evening.


----------



## lazersteve (Aug 16, 2007)

Do you have any chemicals at your disposal?

Steve


----------



## Naitsabes (Aug 16, 2007)

At this point I have muriatic and nitric acid. I can get sulfuric easily.

I have thought of using the muriatic on the deware base to remove the indicated irn first.

Assuming the powder's zirconium and talantalum are oxides I am wondering if simple floatation (panning) might work to remove them thoght it mght require a wettign agent.


----------



## lazersteve (Aug 16, 2007)

I would attack the problem in small samples and find out what works. Maybe cut the metal into several 1" squares and test various acid combinations. Your suggestion about the iron sounds like a decent starting point. I would try *dilute* nitric on one of the samples also. 

Of course the final dissolving will need to be hot AR to get any Gold, Platinum, or Rhodium.

One last possibilty is that the metal is plated and not solid.

Steve


----------



## Naitsabes (Aug 16, 2007)

We thought of the possibility of the sheet being plated - so the surface of the dewar base (I have several of these) was ground before the xray analysis.

But I beleive you are of course right proof will be seen in the digestion.

After using muriatic for the Iron my thought was to remove the gold by one of the auric chlorid methods you describe.

The material with the zirconium and tantalium will be the more difficult as both elements have melting points and behavior in acid much like platinum.

However as I understand both Zr and Ta oxidize readily to readily in the case of zircon - as in bang! - Best work with very small amounts.

The refinner who sent back the powder said the chemist had a hell of time melting and digesting the material which is alos consistant with the analysis.

The black-grey color of the powder suggests oxidation has already occurred. Which is why I am wondering if a mechanical seperation of the Ta and Zr from the Au and Pt might be sucessful?

Of course they may still be alloyed together?

I am also wondering how to best recieve the value from any material I refine off this powder or sheet?

I've quite a bit of gold plated material about - I will probably work the plated material first to get a little practice before I tackel this difficult material.


----------

