samuel-a said:
Chris.
It amaze me time and again, how you (and the other "veterans") seems to have the bigger picture in mind and are willing to share your point of view with such detail. For that i pesonally would like to thank you.
goldsilverpro said:
The easiest and, probably, most accurate way on identical parts (at least, in appearance), such as these, is to fire assay the whole parts separately. To sample them, since they all appear to be identical, I would probably just grab a part here and a part there - I can't see how splitting down the lot by coning and quartering or using a sample splitter would give much improvement. In this case, you can probably run 2 parts per fire assay but, if the total copper and nickel is more than about 2 grams, you may only be able to run 1 part per assay. Since organics are involved, the parts must be incinerated before fluxing. This is easily done by weighing the 2 parts and placing them in an empty assay crucible. Then put them in a hot (say, 1850F) assay furnace, with the door opened just a crack to let in a little oxygen, and burn them until they fall apart into white ash. This might take 45-60 minutes. or more. Occasionally, you might have to pull the crucible out and give it a stir with a small diameter steel rod. If they aren't burned completely and any carbon remains, you'll probably end up with a too large lead button. After incineration, pre-mix the flux in a separate crucible, pour it onto the ash, stir it all up, and run a normal fire assay.
What flux composition will be needed for such material?
According to spec sheets, about 60-70% of package matrix is composed of fused silica with the rest being mostly epoxy of some sort (which wouldn't matter since incinerated)
That's a lot more silica than I expected, but since silica is usually used in assay fluxes, it may not cause a problem unless there is so much that it won't allow the epoxy to burn out. If the silica melts in the 1850F heat and coats the epoxy and prevents it from burning out, you might try incinerating at a much lower temperature - say, 1000F, for a longer period of time. It might also help to crush up the part in a cast iron mortar and pestle before incinerating. This won't work, though, if any of the gold sticks to the cast iron. It probably won't.
You might have to experiment with the flux mixture but, to start with, here's what I would try for these parts.
60-70 g litharge
30 g anhydrous borax or borax glass
20-30 g anhydrous soda ash
Sugar or flour
A little fluorspar (try 2-5 grams) if the molten flux is too thick. If you use too much, the crucible can be severely attacked and you can leak flux onto the furnace floor.
Except for the sugar or flour, the amounts of the ingredients are not that super critical and can vary somewhat.
Bismuth trioxide can be used instead of litharge and is much safer (and more expensive). I haven't used it so I can't comment on it. If you use litharge, make sure you have excellent furnace exhaust. You don't want to breathe that crap.
The purpose of the sugar or flour (I use sugar) is to reduce part of the litharge (lead oxide) to lead metal, which is formed in droplets wherever a sugar particle contacts a litharge particle and these rain down through the mixture to collect the PMs. The remaining unreduced litharge acts as an important part of the flux. The sugar or flour is burned to carbon and that's what reduces the lead. Ideally, about a 25 gram lead button is formed. For the brand of granulated sugar I was using, that took about a level 1/2 teaspoon. Since sugar and flour can vary tremendously, you'll have to experiment with the amount. In general, it takes less flour than sugar. If the epoxy doesn't burn out completely, a lot more lead can be reduced and you may need no sugar or flour at all. If way too much lead is formed, you can either use a huge cupel or split 1 part into 2 pieces and run it in 2 crucibles.
If you're interested in both Au and Ag: cupel the lead button, weigh the Au/Ag bead, wrap the bead in lead foil along with enough silver to give about a 4-6/1 silver/gold ratio, cupel, part, weigh the gold, calculate the silver from the 2 weighings. If you're only interested in the gold: add the silver to the flux mixture, cupel the lead button, part, weigh the gold.
Were I doing this, I would probably run a few experimental assays before settling on the method I would use. The high silica could cause problems and change the whole approach. I sold my assay equipment so I have no way to play with it. Good luck!