Smoking loss is very real. If you let it burn in open container, losses in our hands were as high as 3-7% (in situ formed Pd is so light that slightest air turbulence catch it and carry it away). I don´t know if moistening with water help to somewhat pack it so it does not smoke that badly, never tried to melt it in open container in bulk wet or dry. I did damp and dry batches, on large scale in closed system. It can be managed, but you need to be prepared for big flame show
My favourite way is bigger graphite crucible in induction furnance, where you can very precisely monitor the temperature - as graphite conducts heat pretty well.
And also never forget to set the fumes on fire. These are one of the nastiest fumes I ever encountered. Awful, nauseating, acrid, burnt and persistent smell, it gets onto your tongue and you can even taste that atrocity, for very decent time. I don´t know what is inside them, but as the article points out, HCN can indeed be present - and by the smell (I unfortunately whiffed them few times doing this) I can say it can have cyanide hint to it - like acrid, irritating, little chlorine-like. But I cannot say it for sure. Presence of cyanide can be tested if little bit of the fumes is contained (eg to the PET bottle) and then bubbled through solution containing dissolved iron - blue colour is developed (prussian blue test).
Take the crucible to like 350-400°C and let the heat slowly crawl through the bulk of the material inside. It start to burn on the edges, then going deeper to the center. I usually cover the top of the crucible with two layers of refractory wool and weigh it down so there are no gaps between crucible and wool. Any gaseous product arising would need to pass through the wool - so if any Pd is carried in smoke as ultrafine particles, they will catch on the wool similarly as on the filter paper.
It is very obvious if you are loosing something. When you are done, you can clearly see greyish-purplish-greenish oxidized surface of the wool covered with ultrafine Pd. By peeling the wool layer by layer you see how deep it has penetrated - with bigger batches, or less controlled heating, one 2 cm layer of wool sometimes isn´t enough and you will clearly see how the top of the wool darkens
And that dark stain cannot be burnt away with torch - carbon residue will burn. I also tested this with XRF and Pd indeed crawled this distance through the wool (at least 2 centimeters, batch of ca 100 g, nearly dry, in ca 200-300ml graphite crucible, steadily heated in induction to 350-400 °C on the surface of graphite - till fumes production ceased).
As professional, Lou pointed many good suggestions on how to convert these with minimal losses - by reducing it with hydrogen in tube furnance or similar device. I planned to build one low pressure apparatus precisely for this chore - reduction of platinum and palladium salts to metals, recently acquired some parts, hydrogen cylinder... But everything gone south when I lost my partner and all of the equipent and premises with him :/
Second possibility is to do it wet, by reducing with zinc directly, altough I don´t know how the free oxime would behave. My idea was to dump the complex into basic solution, where it can possibly disintegrate to Pd hydroxide and deprotonated oxime double salt... But I don´t know how it would go in real life conditions. These complexes are fairly stable.
And also never forget to set the fumes on fire. These are one of the nastiest fumes I ever encountered. Awful, nauseating, acrid, burnt and persistent smell, it gets onto your tongue and you can even taste that atrocity, for very decent time. I don´t know what is inside them, but as the article points out, HCN can indeed be present - and by the smell (I unfortunately whiffed them few times doing this) I can say it can have cyanide hint to it - like acrid, irritating, little chlorine-like. But I cannot say it for sure. Presence of cyanide can be tested if little bit of the fumes is contained (eg to the PET bottle) and then bubbled through solution containing dissolved iron - blue colour is developed (prussian blue test).
Take the crucible to like 350-400°C and let the heat slowly crawl through the bulk of the material inside. It start to burn on the edges, then going deeper to the center. I usually cover the top of the crucible with two layers of refractory wool and weigh it down so there are no gaps between crucible and wool. Any gaseous product arising would need to pass through the wool - so if any Pd is carried in smoke as ultrafine particles, they will catch on the wool similarly as on the filter paper.
It is very obvious if you are loosing something. When you are done, you can clearly see greyish-purplish-greenish oxidized surface of the wool covered with ultrafine Pd. By peeling the wool layer by layer you see how deep it has penetrated - with bigger batches, or less controlled heating, one 2 cm layer of wool sometimes isn´t enough and you will clearly see how the top of the wool darkens
As professional, Lou pointed many good suggestions on how to convert these with minimal losses - by reducing it with hydrogen in tube furnance or similar device. I planned to build one low pressure apparatus precisely for this chore - reduction of platinum and palladium salts to metals, recently acquired some parts, hydrogen cylinder... But everything gone south when I lost my partner and all of the equipent and premises with him :/
Second possibility is to do it wet, by reducing with zinc directly, altough I don´t know how the free oxime would behave. My idea was to dump the complex into basic solution, where it can possibly disintegrate to Pd hydroxide and deprotonated oxime double salt... But I don´t know how it would go in real life conditions. These complexes are fairly stable.