Osmium = Os 99.96% pure

10x
The largest piece = 1/8th inch square
Color of metal chips = accurate, except for the shadows and shinny light reflections.

20x
A variety of crystal structures are present.

40x
There is a hint of blue in this intensely deep black color.
Could not get decent images at higher power due to irregular surfaces

30x
Largest fragment = .04” pretty much square
Smallest piece = .02” very irregular surfaces but gestimating about ½ the size of largest.
The largest fragment is used for the lead, silver fusion test.
Took ¼ gram of 99.95% Lead metal and flattened it to accommodate a previously cleaned 0.060” Ag (inquart) prill, along with the approximately 0.04” Os fragment. The Lead was folded twice to totally wrap these inquarts and placed on a cupel to be melted after the cupel is sufficiently heated.

This is the bottom of a previously used cupel. I merely scrape a small depression for the molten lead to reside within and allow the heated cupel to absorb the generated oxidized Lead (liquid litharge).

Driving off the remaining lead contaminating the silver prill.

10x
A dirty green stain surrounding the silver prill.
The Ag prill is obviously not a good sphere.
The silver prill detached from cupel with only minor difficulty, which, according to some assay books suggests no lead remaining. After countless numbers of cupellations I am not convinced that whether or not a silver prill sticks to or is not adhering to cupel is a sign of purity or if any Lead remains.
Cupel too hot to touch.
The hot sublimate colors are fading.
The reddish color where the Silver prill rests changes to brownish then green.

40x
Prill rests upon a glass slide.
No obvious surface oddities, except there is no Ag crystalline pattern indicating to me that the prill is contaminated with something. In this case it is Osmium.
Size of the AgOs prill = .07”
At the 12 o’clock position the Osmium can be seen protruding from the silver.

20x
Bottom of OsAg prill prior to digestion.
The black Osmium can be seen protruding through the silver. Not sure why the silver did not totally encapsulate the osmium.

40x
Bottom of prill
Color of prill = accurate
The black Osmium is not very distinguishable, no clear crystalline structure.
Not able to focus on all portions of an irregular surface.
Bottom of this Ag prill shows how it was attached to cupel surface.

40x
Digesting the prill in 1 part nitric acid and 2 parts water on a glass slide that has a depression (well).
Air bubbles are making the prill move so a out-of-focus image.

40x
Prill still being digested and exposing more and more Osmium.
No specific odor, but there is a slight coffee and vinegar smell I presume the coffee is the silver nitrate, but the vinegar is odd. Osmium, like the other PGM’s is or can be highly reactive and may be catalyzing the HNOx into who knows what?
It appears that not enough silver remains in relationship to the amount of Osmium just after digestion began.
The Os forms a core even though part of the Os was exposed prior to nitric digestion.
The remaining Ag has tiny facets that I have seen before and always thought it was due to trace amounts of Rh.

40x

40x

40x
Semi-careful examination of these last photomicrographs indicate that some Os is actually being etched, creating the ridges. Is this because there was a small amount of silver within the Os or is Os actually being attacked by the HNO3 or more likely the silver nitrate?

40x
The odor at conclusion makes me sneeze and a couple hours after completion I had a very sore throat.

70x
Attempting to illustrate a portion of the Os crystalline surface structure.

50x
The odor at this stage of the Ag + Os digestion makes me sneeze and a couple hours after completion I had a very sore throat. However, I did not experience any eye irritation as Os is reported to do.
Size of remaining Os prill = 0.04”
Apparently, I essentially retrieved all the Os. There are many tiny fragments littering the slide.
I had always heard that Osmium will not alloy nor be found within a silver prill, but only be attached to the bottom of prill, and care must be taken to avoid losing the black specs between cupel and the silver prill. Obviously, these images clearly show that in this instance the silver almost covered all the osmium. In fact, it have covered it all, and my crude torch cupellation vaporized some or enough silver to expose this Osmium.
A thorough microscopic examination of the cupel indicates no particles of silver nor Osmium.
The next test (fusion/cupellation) will be to have a much smaller amount of Os to determine if silver will totally cover the Os and if smaller amounts of Os will alloy with the silver.