A quantity of powdered lead chloride was added to a beaker along with a specific quantity very pure ammonium chloride. These two compounds were intimately mixed. This compost was then heated to dehydration to remove all moisture, and then subjected to slow, careful, sublimation on a hotplate.

The seventh image shows what the sulphur/sal ammoniac looks like when boiled down to wet salts. A few drops of distilled water was added to dissolve everything, and obtain a very dark red oil/sulphur.

The third from last image shows the caput mortuum that was left over after the sublimation process. There was still quite a bit of sal ammoniac that had not sublimed, but this is of no concern. I'm wondering if the dark black/red liquid on top is a more impure version of the same sulphur/sal ammoniac that had not sublimed fully. The bottom salt layer is also interesting. Sparkling crystals are seen. They are dark gray/white. Probably lead chloride.

I didn't start from lead/silver nitrate as Fulcanelli suggested. I started with lead acetate made by boiling lead in hydrogen peroxide + acetic acid. The soluble lead acetate was precipitated with ferric chloride (was very messy). I washed it a number of times, but still ended up with an impure product. The red/brown contaminate was iron (III) acetate. I wish I would've used NaCl to precipitate the lead chloride, but that's experience for you.

I think this particular process is only really worth carrying out on a large scale. Microscale quantities like I'm working with doesn't yield very much.

This work completely destroyed the beaker I was using. The bottom of the beaker was cracked & broken. A probable cause might be related to heat stress, but maybe this was due to another force. The lead chloride/sal ammoniac that touched the sides of the beaker was almost impossible to remove. It was almost as if it had fused with the glass to form a sort of cement. This process is definitely hard on the glassware.

In the last few images we see the caput mortuum. There appears to be a black layer of dark silt like material that somewhat resembles black oil, lead dioxide, or possibly colloidal lead.

Donations go a heck of a long way towards helping out with future projects. A full write-up of this particular process can be purchased on the publications page here: http://www.vitriolum.net/index.php/publications-books-papers.html