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Palladium (Pd)

 

Because I don't have Palladium metal on hand I am forced to make an alloy of Lead metal and 99.9% Palladium Chloride (PdCl) standards.
To accomplish this task I begin by cutting a 1 gram piece of 99.5% Lead from a small bar, which is hammered thin and flat. Then I curl up the outside edges to make what I refer to as a boat, as seen in the below image.

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This image is showing the pipett dispensing a total of 2 ml of liquid palladium chloride into the Lead metal boat.
Each milliliter is supposed to equal 1 mg of Pd.
I suspect that some Pd will be volatilized as the propane torch heats the liquid.
No metal odor was detected as I drove off the liquid, but could certainly smell the chlorine.
Some caution is necessary to avoid melting the thin Lead edges and thus losing liquid.
When all the liquid has been dried the thin Lead is folded in half and folded again and again as shown below. Then this metal that now contains the residue from the liquid is hammered to somewhat seal-in this reside, so that when the lead is melted it will alloy with the Pd.

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These above images are the melting and alloying of the folded Lead boat.
Although these images are taken during the hot stage and will be significantly different when the plaster tablet has cooled they nevertheless provide sublimates of this potential alloy that when compared to Lead alone will be slightly different and provide valuable clues for future reference.

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10x
This image shows the resultant cooled PbPd alloyed button on the above plaster tablet(s).
Colors of this cold plaster tablet and button are close to accurate, excepting shadows and reflective light. Higher magnification was not better.
There are pieces of plaster dust clinging to the button. Apparently I did not thoroughly clean the cavity that holds the button from running around.
Oddly this Lead button does not have the typical red lead oxide blotches, making me a little suspicious as to what might be happening.
Direction of torch flame is from right to left.
This button is significantly different than all the other Lead PGM button. Plus, it is the only LEAD button to have a sprout and may be an anomaly indicative to palladium, because Pd is known to absorb unusually large amounts of hydrogen and give this gas up during cooling.
This button was removed from tablet, reasonably cleaned of adhering plaster and minor slag then cupelled as shown in following images.
Prior to cupelling this button a 20+mg of silver is placed in the cupel and this button resting ontop of the silver to assure that the silver is absorbed by the lead. Although I tried to make all Ag inquarts close to the same size/amount no exacting amounts of was initiated. because the purpose was merely to capture as much of the pgm as possible and examine the results on the final silver bead.

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This and the following images attempt to demonstrate a simple cupellation procedure that anyone can do after a little practice. Thus, there is no immediate need of having expensive electric/gas furnaces to accomplish the normal laboratory setting and task of obtaining precious metal prills from cupelling lead buttons of any size.

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The torch flame and blast force is normally kept where this image demonstrates, which keeps the cupel hot to absorb the molten Lead and not create too much heat actually on the molten button. If too much heat is applied to the button it will boil and spit, and at same time vaporize too much precious metal.
Learning how to do this is merely being willing to take the time of practicing.

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Although this and the below image are fuzzy due to my inability to not move as I click the shutter the images still show a hot (above) and cooler (below) cupel with the alloyed resultant silver prill. Colors change fast as cooling occurs.

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Cupel is not hot to touch and the oxides are now much different in color.

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10x
The alloyed silver prill resting inside the cavity I previously dug into the cupel to contain the original Lead button. Most of the molten lead is absorbed into the boneash cupel and a small amount is vaporized and can be seen a wisp of smoke.
I save the used cupels if they have not been saturated with Lead and whatever contaminates the Lead may contain. Usually, I scrape away any obvious contamination from the surfaces and use these clean areas to conduct tests like this thus avoiding using new cupels. As long as there is a sufficient amount of uncontaminated cupel surface and the cupel does not crumble into a mess while scraping a new surface and cavity for the Lead bead to be cupelled within then small tests like this one works quite well.
Conducting cupellations like this will cause an unavoidable loss of some silver and possibly other precious metals. However, it is a quick and inexpensive way to make reasonably accurate tests without having to resort to constantly relying upon laboratory expertise.

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25x
This magnification clearly illustrates the crystalline structure of the alloyed silver prill.
Colors are a bit dark, but necessary to show in detail the crystalline appearance cause by the presence of Pd in silver.
At this stage I have no way of knowing how much actual Pd is present, but, this image suggests that the bulk of Pd managed to become alloyed.
Normally, according to what I read most Pd deposits contain much less per ton than what this image suggests.
Now that this method of alloying seems to work I will add smaller fractional amounts to exacting quantities of silver to get a handle on bead appearances, which I suspect, based upon much of my previous related efforts will radically change from this image.

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40x
This higher magnified view of the PdAg prill more clearly shows crystalline structure of this type of alloy and should be of significant aid in helping to make educated guesses as to what some precious metal prills might contain.
Because of the curved surface only a portion of this spheroid could be focused.
Color of bead is actually much whiter, but the surrounding cupel colors are masking the steel whiteness.
Naturally, I keep all beads of these tests so i can conduct additional tests, such as dissolving this prill in water/nitric acid bath and using other chemicals (DMG) to prove the presence of Pd.

1-01-07, 5:30PM
The primary purpose of this portion of the assay is to determine what the crystal structure of prill may appear like under the surface, as well as collect any metallic debris.
To be sure that this AgPd prill was as clean as practical it was re-melted by the propane torch flame, which forced a draft directly upon the molten prill driving off any residual Pb. There were traces of Pb.
The bead size measures = .06” (diameter) or the equivalent of approximately 25mg or 25 ounces per ton if 100% silver.
Not visible to naked eye, but at 40x there can be barely seen hundreds of tiny white metal spheres left in cupel cavity where the prill was re-melted. This indicates that the torch blast was too strong, or that this PdAg alloy when melted may be spitting, which is a phenomena that I will have to try to examine. In addition there was a green cupel stain further suggesting absorption of the alloy into the cupel, which is a bad sign and demands investigation.
While digesting this prill in nitric acid and chlorine free distilled water and heating till vapors rose there was a unique odor, but different than the strong coffee odor that AgRh in same type solution produces.

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40x
No heat applied after 10 minutes submerged in the acidic solution.

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40x
5:55PM -- Could not focus well because the digestive action of air bubbles kept moving the prill; but primary reason for this image was to capture the yellow solution color.
The liquid color on the surface edge of prill is a lime-green, whereas the old chemistry books claim this parting-action of a PdAg bead will be brown.

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40x
Same as above image, but focusing on glass surface which these small, blackish crystals that have been cast off the prill and are resting upon & within the well (concave part of glass slide).
Surface of prill is turning dark and becoming black.
Color of solution is influencing over-all image.

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40x
Due to the large diameter of this prill, it failed to be totally submerged, causing the portion above the acid/water to form the yellow-green crystalline mass near top of prill.

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50x
6:40PM and only partially digested, but not much heat has been applied to the glass slide.

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50x
6:40PM and only partially digested, but not much heat has been applied to the glass slide.

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70x
Some of the un-dissolved prill debris, which eventually dissolves.
The lemon yellow solution color is strongly influencing the color of these metal fragments.

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50x
As the solution gets saturated complex nitrate crystals of Pd & Ag form along the outer edges of the pregnant solution and eventually cover the entire area as the solution dries.

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50x
Due to evaporation -- Orange-yellow transparent crystals forming along the perimeter of solution. These crystals are silver nitrate and some type of palladium/silver nitrate/water complexation.
This simple 1 part HNO3 & 4 parts H2O completely dissolved this PdAg alloy.